JP2002503761A - Tablets containing bleach - Google Patents

Abstract

  (57) [Summary] The present invention discloses a detergent / detergent compact comprising a bleach. This molded body is characterized by having a high hardness and a high disintegration rate by using a bleach having an average particle size of more than 0.4 mm. Preferably, the bleach contains less than 0.4 mm particles in an amount of less than 30% by weight.

Description

DETAILED DESCRIPTION OF THE INVENTION

TECHNICAL FIELD The present invention relates generally to detergent / detergent tablets (bleaching tablets) containing a bleaching agent.
About. More particularly, the present invention relates to tablets containing bleach, such as laundry detergent tablets, dishwasher detergent tablets, bleach tablets, water softener tablets and the like.

[0002] Detergent / cleaning compositions in the form of tablets are well known in the art and have been widely disclosed in the prior art. However, tablets have not been particularly successful in the market. The reason for this is that, despite the various advantages of tablets, they have drawbacks that adversely affect the manufacture and use thereof, and the feeling of use by consumers. The key advantages of tablets are that they eliminate the need for consumers to weigh product doses, and that high density reduces packaging and shipping costs, as well as aesthetics. (This advantage should not be underestimated), but these advantages are offset by the following disadvantages: That is, tablets have conflicting problems between acceptable hardness and sufficient disintegration / dissolution rates, and a number of technical problems in tablet manufacturing and packaging.

[0003] In particular, the conflicting problem that exists between sufficient tablet hardness and a sufficient rate of dissolution is a central issue. Tablets with sufficient stability (ie, dimensional stability) and puncture resistance can only be manufactured by applying relatively high pressure, and the components in the tablet are subjected to a large compressive force. In addition, the disintegration of the tablet into the washing liquid is delayed, resulting in an excessively delayed release of the active substance during the washing and washing process.

[0004] The too long disintegration phenomenon of tablets has another disadvantage. That is, the conventional laundry detergent / washing product tablet cannot be washed out of the detergent input room of the home washing machine into the washing process. This is because such tablets cannot be disintegrated at a sufficiently fast rate into small secondary particles that are small enough to be washed out of the washing machine into the washing tub.

[0005] As described above, tablet hardness (ie, transport / handling stability) and easy disintegration of tablets are conflicting problems, and in order to solve this problem,
A number of solutions have been attempted in the prior art. One solution is that which is known in particular in the pharmaceutical field, but has also been extended to the field of laundry detergent / detergent product tablets. According to this solution, certain disintegrants are incorporated into the tablet, which promotes water intrusion and, upon contact with water, causes swelling, gas foaming and disintegrating effects. Is shown. Other solutions have been proposed in the patent literature,
Tableting of a premix having a predetermined particle size, separation of certain components from other components,
Coating of each component or the whole tablet with a binder is disclosed.

For example, EP-A-0 522 766 (Unilever) discloses tablets of a compressed, granular laundry detergent composition, which comprises a surfactant, a builder, and a cellulosic disintegrant. And at least some of the particles are coated with a disintegrant. This disintegrant exerts both a binder action and a disintegrant action when the tablet is dissolved in water. This reference points out the overall difficulty in producing tablets that combine sufficient stability with effective solubility. In this case, it is disclosed that the particle size of the mixture to be tableted exceeds 200 μm, and the difference between the upper limit and the lower limit of each particle size is 700 μm or less.

[0007] Patent documents relating to the production of detergent tablets include EP-A-0 716 144 (Unilever).
) And EP-A-0 711 827 (Unilever), wherein the former discloses a tablet having an outer shell of a water-soluble material, the latter comprising as an ingredient a citrate having a predetermined solubility. Is disclosed.

[0008] EP-A-0 711 828 (Unilever) discloses a tablet for laundry detergent using a binder (especially polyethylene glycol) which can exert a disintegrating action if desired.
This detergent tablet is produced by tableting the granular laundry detergent composition at a temperature of 28 ° C. to the melting point of the binder material, and this tableting treatment is always carried out at a temperature lower than the melting point. According to the disclosure of the examples of the patent document, if the tableting process is performed at a high temperature, the tablet manufactured by the method disclosed in the patent document can have high breaking strength.

[0009] Detergent tablets, in which each component is present separately from the other components, are disclosed in particular in EP-A-0 481 793 (Unilever). The detergent tablets disclosed in this document contain sodium percarbonate in a state separated from all other components that may affect its stability.

None of the above prior art documents disclose the importance of the physical properties of each component, especially the physical properties of the bleach, to the detergent tablet. In addition, any prior literature,
By selecting and using a bleaching agent having a predetermined particle size range, the detergent /
There is no disclosure of improving the solubility of the detergent tablet.

The problem to be solved by the present invention is to provide a bleach-containing detergent tablet which combines high hardness with excellent disintegration properties. Even when the detergent tablet provided by the present invention is charged from the detergent charging chamber, almost all the detergent can be washed out into the washing liquid without leaving the detergent in the detergent charging chamber. Besides such special detergent tablet properties, the detergent tablets of the present invention can have excellent cleaning properties.

SUMMARY OF THE INVENTION Accordingly, the present invention is directed to a compressed granular detergent / detergent detergent / detergent tablet comprising a bleach, a builder and optionally other detergent / detergent components, wherein the bleaching agent Provides a tablet characterized by having an average particle size of greater than 0.4 mm.

The term “average particle size” as used herein refers to a calculated value obtained by (content ratio of sieving fraction) × (mesh width of sieve). For example, when extremely small particles and extremely large particles are mixed, individual values for which such an average value is calculated may be spread over a wide range. However, in accordance with the present invention, the bleach has a relatively narrow particle size distribution such that it does not have a broad particle size distribution, but exists near the average. In particular, so-called fine particles must be removed as far as possible, so that in the preferred detergent tablets of the invention, the bleaching agent is characterized by being substantially free of particles with a particle size of less than 0.2 mm. I do.

The term “substantially free” as used herein means a content of less than 2% by weight, preferably less than 1% by weight, more preferably less than 0.5% by weight.

According to the present invention, bleach dust and particulates are not only as absent as possible, but also such that the content of particles whose particle size is less than 0.4 mm is also as small as possible. Should be maintained. Thus, according to one preferred embodiment of the invention, the bleaching agent reduces particles having a particle size of less than 0.4 mm to less than 30% by weight, preferably less than 20% by weight,
More preferably, it is present in an amount of less than 10% by weight.

Therefore, the content of bleach particles having a relatively large particle size must be as large as possible. According to one preferred embodiment of the invention, the bleach particles have a particle size not only exceeding 0.4 mm, but also distinctly larger, for example greater than 0.8 mm. According to one preferred embodiment of the invention, the bleaching agent is used to reduce particles having a particle size of more than 0.8 mm in an amount of more than 10% by weight, preferably more than 20% by weight, more preferably 30% by weight In excess of

Nevertheless, bleach should not, of course, be incorporated in the detergent tablets of the present invention in the form of large chunks. From a practical point of view, bleach particle sizes of less than 2.0 mm have been shown to be effective, and the bleach present in the detergent tablets preferably has a particle size of greater than 1.6 mm. Is not substantially contained.

Bleaching Agents, Bleaching Activators and Bleaching Catalysts To provide the required bleaching performance, the detergent tablets of the present invention contain one or more bleaching agents. Among the bleaching compounds that produce hydrogen peroxide (H ₂ O ₂ ) in water, sodium perborate tetrahydrate and sodium perborate monohydrate are:
Of particular importance. Other useful bleaching agents are, for example, sodium percarbonate, peroxypyrophosphate, citrate perhydrate and hydrogen peroxide producing persalts or peracids, such as perbenzoates, peroxophthalates, Diperazellaic acid, phthaloiminoperic acid or diperdocanedioic acid.

Further, according to the detergent tablet of the present invention, the content of the bleaching agent can be changed according to a desired product. The typical content is 5 to 50% by weight, preferably 10 to 40% by weight, more preferably 15 to 35% by weight, based on the total amount of the tablet.

As mentioned above, the bleach content of the tablet depends on the intended use of the tablet. Representative tablet form heavy duty detergents contain bleach in an amount of 5 to 30% by weight, preferably 7.5 to 25% by weight, more preferably 12.5 to 22.5% by weight. Include in quantity. Bleach tablets or bleach accelerator tablets contain bleach in an amount of 15 to 50% by weight, preferably 22.5 to 45%.
It is contained in an amount of 30% by weight, more preferably in an amount of 30% by weight to 40% by weight.

According to the invention, particularly preferred bleaches are sodium perborate and sodium percarbonate, with sodium perborate monohydrate being particularly preferred.

In addition to the bleaching agents described above, the detergent tablets of the present invention can include a bleaching activator. To improve the bleaching effect when washing at a temperature of 60 ° C. or lower, a bleach activator can be incorporated. Bleaching activators that can be used include perhydrolysis (
A perhydro lysis) conditions, aliphatic peroxocarboxylic acids, preferably C _{1 ~ 10} (
Preferably a compound so as to form a C _{2 ~ 4)} aliphatic peroxocarboxylic acids and / or unsubstituted or substituted perbenzoic acid. Substances containing O- and / or N-acyl groups and / or unsubstituted or substituted benzoyl groups having the stated number of carbon atoms are preferred. Suitable bleach activators include polyacylated alkylenediamines, especially tetraacetylethylenediamine (TAED), acylated triazine derivatives, especially 1,5-diacetyl-2,4-dioxohexahydro-1,3,5-triazine (DADHT) ), Acylated glycolurils, especially tetraacetylglycoluril (TAGU), N-acylimides, especially N-nonanoylsuccinimide (NOSI), acylated phenolsulfonates, especially n-nonanoyl or isononanoyloxybenzenesulfonate (n- or iso-NOBS), carboxylic anhydrides, especially phthalic anhydride, acylated polyhydric alcohols, especially triacetin, ethylene glycol diacetate, and 2,5-diacetoxy-2,5-hydrofuran.

In addition to or instead of the usual bleach activators, so-called bleach catalysts can be introduced into the tablets according to the invention. A bleach catalyst refers to a transition metal salt or a complex of a transition metal that enhances the bleaching action, such as a manganese-, iron-, cobalt-, ruthenium- or molybdenum-selenium complex or carbonyl complex. In addition, manganese complexes, iron complexes, cobalt complexes, ruthenium complexes, molybdenum complexes, titanium complexes, vanadium complexes, copper complexes and the like containing a nitrogen-containing tripod ligand, and cobalt-, iron-, copper- and ruthenium- Amine complexes can also be used as bleach catalysts.

The tablet of the present invention may contain 0.5 to 30% by weight, preferably 1%, based on the total amount of the tablet.
It contains -20% by weight, more preferably 2-15% by weight, of one or more bleach activators or bleach catalysts. Such dosages can vary depending on the use envisioned for the detergent tablet. That is, in a typical heavy duty detergent tablet, the content of the bleaching activator is usually 0.5 to 10% by weight, preferably 2 to 8% by weight, more preferably 4 to 6% by weight. Drug tablets contain higher amounts, for example, 5-30% by weight, preferably 7.5-25% by weight, more preferably 10-20% by weight. Those skilled in the art can freely carry out the formulation without limitation, and by changing the content of the bleaching activator and the bleaching agent, a relatively strong bleaching action to a relatively weak bleaching action can be achieved. Laundry detergent tablets, detergent tablets or bleach tablets can be produced as having.

A particularly suitable bleach activator is N, N, N ′, N′-tetraacetylethylenediamine, which is widely used as a detergent component. Accordingly, suitable detergent / detergent tablets contain such a tetraacetylethylenediamine as a bleach activator in the amounts described above.

Builders, Surfactants and Disintegrants In addition to the ingredients described above, the detergent tablets of the present invention may contain other ingredients in amounts determined by the intended use of the tablet. That is, substances selected from the group consisting of surfactants, builders and polymers are particularly suitable for use in the tablets of the present invention. One skilled in the art can easily select each component and its dose without difficulty. For example, heavy duty detergents contain relatively high amounts of surfactant, while bleach tablets may not contain any surfactant. Builder doses can also vary depending on the intended use.

Builders According to the detergent / detergent tablets of the invention, any builder commonly used in detergents / detergents can be used, in particular zeolites, silicates, carbonates, organic cobuilders. Phosphates can be used as well, as long as they are not ecologically damaging.

A suitable crystalline layered sodium silicate has the formula: Na ₂ MSi _x O _{2x + 1} yH ₂ O. Wherein M is sodium or hydrogen, x is a number from 1.9 to 4, y is a number from 0 to 20, and a preferred value for x is 2, 3 or 4. Crystalline sheet silicates of this kind are described, for example, in European Patent Application EP-A-0 164 514. Preferred crystalline layered silicates of the above formula are those wherein M is sodium and x is a number of 2 or 3. Particularly preferably, both β- and δ-sodium silicates of the formula Na ₂ Si ₂ O ₅ yH ₂ O are used, and β-sodium silicate can be obtained by methods described in the literature. (See, for example, WO-A-91 / 08171).

Other useful builders include a factor (ratio of Na ₂ O: SiO ₂ ) of about 1: 2 to about 1: 3.3, preferably about 1: 2 to 1: 2.8, more preferably about 1: 2. Amorphous sodium silicate having a 2-1: 2.6, which exhibits multiple wash cycle properties due to delayed dissolution. In the prior art amorphous sodium silicate, delayed dissolution can be obtained in various ways, such as surface treatment, compounding treatment, compression or overdrying. The term "amorphous" as used herein refers to X-ray amorphous. That is, the silicate is X
In a line diffraction experiment, it did not show any sharp X-ray reflections typical of crystalline materials,
At best, they show only one or more maxima of scattered X-rays with a range of diffraction angles of several degrees. However, particularly good builder properties can be achieved in electron diffraction experiments, even when the silicate particles form a bent or sharp diffraction maximum. This means that the size of the product crystallite area is 10 to several hundred n
m (up to 50 nm), the dimensions of which are particularly preferably up to 20 nm. Such so-called X-ray amorphous silicates exhibiting dissolution properties which are slower than ordinary water glass are described in DE-A-44 00 024. Compressed amorphous silicates, compounded amorphous silicates and overdried X-ray amorphous silicates are particularly preferred.

The synthetic zeolite containing microcrystals and bound water that can be used in the present invention is preferably zeolite A and / or P. Commercially available zeolite MAP® (Crosfield)
Is a particularly preferred zeolite P. However, zeolites X and mixtures of zeolites A, X and / or P are also suitable. A eutectic of zeolite X and zeolite A (about 80% by weight of zeolite X) is also suitable for the present invention, for example, as a commercial product (VEGOBOND AX®, CONDEA Augusta S. p. A.) And the formula:
_{nNa 2 O · (1-n} ) k 2 O · Al 2 O 3 · (2-2.5) SiO 2 · (3.5-5.5) represented by H ₂ O.

Zeolites can be used as builders in granular compound compositions and also as powdering agents for the mixture itself to be compressed. Usually, zeolites are incorporated into the premix in these two aspects. Suitable zeolites are
It has an average particle size of less than 10 μm (volume distribution measured by the Coulter Counter Method) and preferably contains 18 to 22% by weight, more preferably 20 to 22% by weight of bound water.

The known phosphates can, of course, be used as builder substances if they are ecologically sound. Preferred phosphate builders are sodium salts such as orthophosphoric acid and pyrophosphoric acid, and particularly preferred phosphate builders are sodium salts of tripolyphosphoric acid.

The dose of the builder is generally between 10 and 70% by weight, preferably between 15 and 60% by weight, more preferably between 20 and 50% by weight. As mentioned above, the amount of builder used depends on the intended use, and bleach tablets are used, for example, at the dose of detergent tablets (usually 10-50% by weight).
Builder (e.g., 20-70% by weight, preferably 25-65% by weight, more preferably 30-55% by weight), preferably 12.5-45% by weight, more preferably 17.5-37.5% by weight. %
).

Useful organic builders are provided that they are ecologically safe for use, for example:
Useful polycarboxylic acids (eg in the form of the sodium salt), examples of carboxylic acids include citric acid, adipic acid, succinic acid, glutaric acid, tartaric acid, benzenehexacarboxylic acid, saccharide acids such as gluconic acid, aminocarboxylic acid Acids, nitrilotriacetic acid (NTA) and mixtures thereof. Suitable salts are those of polycarboxylic acids, examples of carboxylic acids include citric, adipic, succinic, glutaric, tartaric, saccharide acids and mixtures thereof.

Surfactants Suitable detergent / detergent tablets may further comprise one or more surfactants.

The detergent / detergent tablet of the present invention exhibits an anionic,
Non-ionic, cationic and / or amphoteric surfactants and mixtures thereof can be included. From the viewpoint of performance, a mixture of an anionic surfactant and a nonionic surfactant is preferred. The total surfactant content of the tablet is
It is 5 to 60% by weight, preferably more than 15% by weight, based on the total amount of the tablet.

Anionic surfactants Suitable anionic surfactants are, for example, sulfonate type surfactants and sulfate ester type surfactants. Suitable anionic surfactants of the sulfonate type are preferably C ₉ -C ₁₃ alkylbenzene sulfonates, olefin sulfonates (ie a mixture of alkene sulfonates and hydroxyalkane sulfonates),
And a disulfonic acid salt, which may, for example, using a C ₁₂ -C ₁₈ monoolefins having a double bond at the internal and terminal, which was sulfonated with sulfur trioxide gas, then the resulting sulfonation products The product can be obtained by alkali hydrolysis or acid hydrolysis. Other suitable sulfonate-type surfactants, with C ₁₂ -C ₁₈ alkanes,
This is, for example, an alkane sulfonate obtained by sulfochlorination or sulfonation followed by hydrolysis or neutralization. Further, esters of α-sulfofatty acids (ester sulfonates) such as hydrogenated coconut oil, palm kernel oil or tallow fatty acid α
-Sulfonated methyl esters are also suitable.

[0038] Another suitable anionic surfactant is a sulphonated fatty acid glycerol ester. As used herein, the term "fatty acid glycerol ester" is obtained by esterifying monoglycerol with 1-3 mol of fatty acids or transesterifying triglycerol with 0.3-2 mol of glycerol. Such monoesters, diesters and triesters and mixtures thereof. Suitable sulfonated fatty acid glycerol esters are the sulfonation products of C _{6 ~ 22} saturated fatty acids, as the saturated fatty acids include caproic acid, caprylic acid,
Examples thereof include capric acid, myristic acid, lauric acid, palmitic acid, stearic acid, and behenic acid.

Suitable alkyl (alkenyl) sulfates are the alkali metal salts, especially the sodium salts, for the sulfuric acid semiesters of fatty alcohols,
C ₁₂ -C ₁₈ fatty alcohols, for example, coconut oil fatty alcohols, tallow fatty alcohol, lauryl, myristyl, cetyl or stearyl alcohol and the like,
Further, C ₁₀ -C ₂₀ oxo alcohols and secondary alcohols having the same chain length are exemplified.
Other suitable alkyl (alkenyl) sulphates are those having the above-mentioned chain length and containing synthetic straight-chain alkyl chains of petrochemical systems and exhibiting similar disintegration behavior to the corresponding compounds of fat and oil chemistry raw material systems. It is. C ₁₂ -C ₁₆ alkyl sulfates, C ₁₂ -C ₁₅ alkyl sulfates and C ₁₄ -C ₁₅ alkyl sulfates are especially preferred in view of the washing performance. Other suitable anionic surfactants are 2,3-alkyl sulfates, for example,
It can be manufactured by the method described in US 3,234,258 or US 5,075,041 and has the registered trademark DAN (S
hell Oil Company).

Also, a linear or branched chain ethoxylated with 1 to 6 mol of ethylene oxide (EO)
Sulfuric acid monoesters of C ₇ -C ₂₁ alcohols, such as sulfuric acid monoesters of 2-methyl branched C ₉ -C ₁₁ alcohols (EO average 3.5 mol) or C ₁₂ -C ₁₈ fatty alcohols (EO1
~ 4 mol) are also suitable. Due to their high foaming capacity, such surfactants are used only in relatively small doses in detergents, for example in doses of 1 to 5% by weight.

[0041] Other suitable anionic surfactants are salts of alkyl sulfosuccinates, which are also known as sulfosuccinates or sulfosuccinates. The surfactant comprises a sulfosuccinic acid and an alcohol (preferably a fatty alcohol, especially an ethoxylated fatty alcohol).
And a monoester and / or a diester. Suitable sulfosuccinates, C ₈ -C ₁₈ fatty alcohol residues or mixtures thereof are exemplified. Particularly preferred sulfosuccinates comprise fatty alcohol residues derived from ethoxylated fatty alcohols, which, by themselves, can also be referred to as nonionic surfactants (see description below). And). Of these sulfosuccinates, those whose fatty alcohol residues are obtained from a narrow range of ethoxylated fatty alcohols are particularly preferred. Alkyl (alkenyl) succinic acids having preferably an alkyl (alkenyl) chain having 8 to 18 carbon atoms and salts thereof can also be used.

Other suitable anionic surfactants are, in particular, soaps. Particularly suitable soaps are those of saturated fatty acids, such as salts of lauric, myristic, palmitic, stearic, hydrogenated erucic and behenic acids, and especially natural fatty acids,
For example, soap mixtures obtained from coconut oil, palm kernel oil or tallow fatty acids.

The anionic surfactant, including the soap, can be in the form of a sodium, potassium or ammonium salt, and can be in the form of a soluble salt of an organic base such as mono, di or triethanolamine. The anionic surfactant can preferably be present in the form of a sodium and / or potassium salt, particularly preferably in the form of a sodium salt.

Nonionic surfactants Suitable nonionic surfactants are alkoxylated (preferably ethoxylated) alcohols, especially primary alcohols. It consists preferably of alcohols having 8 to 18 carbon atoms and an average of 1 to 12 mol of ethylene oxide (EO) per mol of alcohol,
The alcohol residue may be straight-chain or suitably 2-methyl-branched, or may have a mixture of straight-chain and methyl-branched groups as in conventional oxo alcohol residues. However, alcohol ethoxy having linear groups of naturally occurring _C12-18 alcohols (eg coconut fatty alcohol, palm oil fatty alcohol, tallow fatty alcohol or oleyl alcohol) and an average of 2 to 8 EO per mole of alcohol Rates are particularly preferred. Suitable ethoxylated alcohols include, for example, C _12-14 alcohol + 3EO or 4EO, C _9-11 alcohol + 7EO,
C _13-15 alcohol + 3EO, 5EO, 7EO or 8EO, C _12-18 alcohol + 3EO, 5 EO or 7 EO, and mixtures thereof (e.g., a C _12-14 alcohol + 3EO, a mixture of C _12-18 alcohol + 7 EO) is exemplified Is done. The degree of ethoxylation is a statistical mean, which may be an integer or a fraction for a particular product. Suitable alcohol ethoxylates have a narrow homolog distribution (narrow range ethoxylates, NR
E). In addition to such nonionic surfactants, fatty alcohols having an EO greater than 12 as described above may also be used. An example is (tallow) fatty alcohol + 14EO
, 16EO, 20EO, 25EO, 30EO or 40EO.

In addition, examples of additional nonionic surfactants include alkyl glycosides represented by the formula: RO (G) _x . In the formula, R is a primary, linear or methyl-branched (particularly, 2-methyl-branched) aliphatic group (having 8 to 22, preferably 12 to 18 carbon atoms);
It is a glucose unit having 5 or 6 carbon atoms (preferably a glucose unit). The degree of oligomerization x indicates the distribution of monoglycosides and oligoglycosides, and is a numerical value of 1 to 10, preferably 1.2 to 1.4.

Other suitable non-ionic surfactants can be used alone or in combination with other surfactants and can be alkoxylated, preferably ethoxylated or ethoxylated / propoxylated fatty acid alkyl esters (preferably 1 to 4 carbon atoms in the alkyl chain), particularly fatty acid methyl esters (for example, esters described in Japanese Patent Application No. 58/217598, preferably esters prepared by the method described in WO-A-90 / 13533). .

Further, amine oxide type nonionic surfactants are also suitable, and examples thereof include N-cocoalkyl-N, N-dimethylamine oxide and N-tallowalkyl-N, N-dihydroxyethylamine oxide, In addition, nonionic surfactants of the fatty acid alkanolamide type are also suitable. The dose of such non-ionic surfactant is preferably lower than the dose of ethoxylated fatty alcohol, more preferably less than half.

Another suitable surfactant is a polyhydroxy fatty acid amide represented by the following formula (I).

Embedded image In the above formula, RCO is an aliphatic acyl group having 6 to 22 carbon atoms, R ¹ is hydrogen, an alkyl group or a hydroxyalkyl group having 1 to 4 carbon atoms, and [Z] is 3 to 10 carbon atoms / the number of hydroxyl groups.
3 to 10 linear or branched polyhydroxyalkyl groups. Polyhydroxyfatty acid amides can be obtained by reductive amination of reducing sugars with ammonia, alkylamines or alkanolamines, followed by acylation with fatty acids, fatty acid alkyl esters or fatty acid chlorides.

As a group of polyhydroxy fatty acid amides, compounds represented by the following formula (IV) are exemplified.

Embedded image In the above formula, R is a linear or branched alkyl or alkenyl group having 7 to 12 carbon atoms,
R ¹ is a linear, branched or cyclic alkyl or aryl group having 2 to 8 carbon atoms,
R ² is a linear, branched or cyclic alkyl group or aryl group or oxyalkyl group having 1 to 8 carbon atoms, preferably a C ₁ -C ₄ alkyl group or a phenyl group, and [Z] is an alkyl chain A linear polyhydroxyalkyl group substituted by at least two hydroxyl groups, or an alkoxylated (preferably ethoxylated or propoxylated) derivative thereof.

Suitably, [Z] may be obtained by reductive amination of a reducing sugar (eg, glucose, fructose, maltose, lactose, galactose, mannose or xylose). The N-alkoxy or N-aryloxy-substituted compound is then converted to the desired polyhydroxy fatty acid amide by reacting it with a fatty acid methyl ester in the presence of an alkoxide as a catalyst, for example according to International Patent Application WO-A-95 / 07331. can do.

According to the present invention, suitable detergent / detergent tablets are tablets containing anionic and nonionic surfactants. From a performance point of view, these surfactants are advantageously used in a predetermined ratio.

For example, in a particularly preferred detergent / detergent tablet, the ratio of anionic surfactant / nonionic surfactant is from 10: 1 to 1:10, preferably 7.5: 1 to 1: 5, More preferably, it is 5: 1 to 1: 2.

Advantageously, from a performance point of view, certain surfactants are not present in certain phases of the tablet or in the whole tablet (ie all phases). According to one particularly preferred embodiment of the invention, at least one phase of the tablet does not comprise a non-ionic surfactant.

In the opposite mode, a positive effect can be obtained by allowing a predetermined surfactant to be present in each phase of the tablet, that is, in all phases. The introduction of the above-mentioned alkylpolyglycosides has proven to be particularly advantageous. Thus, preferred detergent / detergent tablets have at least one phase containing an alkyl polyglycoside.

As with the non-ionic surfactants, the absence of the anionic surfactant in each or all phases can result in tablets more suitable for certain applications. Thus, according to the invention, detergent / detergent tablets in which at least one phase is free of anionic surfactant are also possible.

[0056] According to the disintegrant present invention, disintegrant (for so-called tablet disintegrators) was incorporated into the high-compression tablet, to promote disintegration of the tablet, it is possible to shorten the disintegration time. Reference [Roempp (9th edition, Vol. 6, p. 4440) and Voight "Lehrbuch der pharma
According to Zeutischen Technologie "(6th edition, 1987, pp. 182-184), tablets or disintegrants can rapidly disintegrate tablets into water or gastric juice to absorb pharmaceutically active ingredients. It is an auxiliary agent for releasing in a suitable form.

The disintegrant as described above can increase its capacity by invasion of water. That is, on the one hand the volume of the disintegrant itself is increased (swelling) and on the other hand a pressure is created by the release of gas, which causes the tablet to disintegrate and form relatively small particles. A well-known disintegrant is the carbonate / citric acid system, but other organic acids can be used. Swellable disintegrants are, for example, synthetic polymers such as polyvinylpyrrolidone (PVP) or natural polymers and / or modified natural substances, such as cellulose and starch and their derivatives, alginate or casein derivatives.

[0058] Suitable tablets for laundry detergents or cleaning products contain one or more disintegrants, the dosage of which is 0.5 to 10% by weight, preferably 3%, based on the tablet weight. 77% by weight, especially 4-6% by weight.

According to the present invention, suitable disintegrants mean cellulosic disintegrants. Accordingly, suitable detergent / detergent tablets comprise this type of cellulosic disintegrant, the dosage of which is 0.5 to 10% by weight, preferably 3 to 7% by weight, in particular 4 to 6% by weight. is there. Pure cellulose has the empirical formula: (C ₆ H ₁₀ O ₅ ) _n , formally called cellobiose β-1,4-polyacetal, and is composed of two glucose molecules. Suitable celluloses are composed of about 500 to 5,000 glucose units, and thus have an average molecular weight of 50,000 to 500,000. According to the present invention, cellulose derivatives starting from cellulose and obtained by a polymerization analog reaction can also be suitably used as the cellulosic disintegrant. Examples of such a chemically modified cellulose include an esterification or etherification reaction product obtained by substituting a hydrogen atom of hydroxy. However, cellulose in which a hydroxy group is substituted by a functional group to which an oxygen atom is not bonded can also be used as a cellulose derivative. Examples of this group of cellulose derivatives include alkali metal cellulose, carboxymethyl cellulose (CMC), cellulose esters and ethers, and aminocellulose.

The above-mentioned cellulose derivative is preferably used in the form of a mixture with cellulose, without being used alone as a cellulosic disintegrant. The content of the cellulose derivative in the mixture is preferably less than 50% by weight, more preferably less than 20% by weight, based on the cellulosic disintegrant. According to a particularly preferred embodiment, pure cellulose without cellulose derivatives is used as cellulosic disintegrant.

The cellulose used as disintegrant is preferably not used in particulate form, but instead may be granulated or compressed before it is mixed with the premix to be compressed. To a relatively coarse particle form. The detergent / detergent tablets contain the disintegrant in granular form or optionally in co-granulated form as described in the following literature: DE 197 09 991 (Stefan Herzog), DE 197 10 254 (Henkel) and
PCT / EP 98/1203 (Henkel). These references disclose details about the preparation of granulated, compressed or co-compressed cellulose disintegrants. The particle size of such disintegrants is
At least 90% by weight thereof usually exceeds 200 μm, preferably 300 to 1,600 μm, especially 400 μm.
It is in the range of 1,1,200 μm. The relatively coarse particle cellulose-based disintegrants described in the present specification and the above-mentioned patent documents are suitable for use as the disintegrant of the present invention, and these are commercially available products (for example, registered trademark: Arbocel TF-30). -HG, Rettenmaier).

Further, microcrystalline cellulose can be used as a cellulosic disintegrant or one component of the disintegrant. This microcrystalline cellulose can only attack the amorphous regions and completely dissolve the amorphous regions, while partially hydrolyzing the cellulose under conditions that do not alter the crystalline regions (about 70%) ( About the total weight of cellulose
30%). Subsequent non-agglomeration of the microcrystalline cellulose formed by the hydrolysis results in microcrystalline cellulose having a primary particle size of about 5 μm, which can be compressed to particles having an average particle size of 200 μm, for example.

The detergent / detergent tablets of the present invention comprise a disintegrant, preferably a cellulosic disintegrant, preferably in granular, co-granulated or compressed form, wherein the dosage of the disintegrant is Based on 0.5 to 10% by weight, preferably 3 to 7% by weight, especially 4 to 6% by weight.

Other Detergent / Detergent Components In addition to the bleach, bleach activator, builder, surfactant and disintegrant components described above, the detergent / detergent tablets of the present invention relate to detergent / detergent compositions, Other exemplary components can include dyes, fragrances, optical brighteners, enzymes, antifoams, silicone oils, anti-redeposition agents, discoloration inhibitors, dye transfer inhibitors Selected from the group consisting of agents and anticorrosives.

Dyes According to the present invention, the detergent tablets of the present invention can be colored with a suitable dye to improve the aesthetic appearance of the tablets. Suitable dyes can be selected without difficulty by those skilled in the art, which exhibit high storage stability, are not adversely affected by other ingredients and light in the tablet detergent, and have a It does not show significant dyeability and therefore does not dye such fibers.

According to the present invention, any dye which can be oxidatively decomposed in the washing process and a mixture of such a dye with a blue dye (so-called bluing agent) are preferably used in the tablet of the present invention. Can be used. Soluble in water-soluble or liquid organic substances (
It has been found to be advantageous to use a dye (at room temperature). Suitable dyes are, for example, anionic dyes, for example anionic nitroso dyes. One possible dye is, for example, naphthol green (Color Index (CI), Part 1: Acid Green 1, Part 2: 10020) (commercially available, for example, BASF (Ludwig)
Shafen) (commercially available as Basacid® Gruen 970) and mixtures of the dyes with suitable blue dyes. Other suitable dyes are shown below: Pigmosol® Blau 6900 (CI74160), Pigmosol® Gruen 8730 (CI74260), Basonyl (
(Registered trademark) Rot 545FL (CI45170), Sandolan (registered trademark) Rhodamin EB400 (CI45100), Ba
sacid® Gelb 094 (CI47005), Sicovit® Patentblau 85E131 (CI42
051), Acid Blue 183 (CAS12217-22-0, CI Acid Blue 183), Pigment Blue 15 (CI741
60), Supranol® Blau GLW (CAS12219-32-8, CI Acid Blue 221), Nylosan® Gelb N-7GL SGR (CAS61814-57-1, CI Acid Yellow 218), and / or S
andolan® Blue (CI Acid Blue 182, CAS 12219-26-0).

In choosing a dye, it is important to ensure that the dye does not have excessive affinity for the surface of the textile, especially for the surface of synthetic fibers. Another factor to consider in choosing an appropriate dye is that the dyes have different stability to oxidation. Generally speaking, water-insoluble dyes are more stable to oxidation than water-soluble dyes. The concentration of the dye in the detergent varies according to its solubility, and thus oxidation sensitivity. Was dissolved in water easily dyes, e.g., the above-mentioned Basacid (R) Gruen and Sandolan (TM) For Blue, a dye concentration in the range of a few 10 ^-2 to 10 ^-3% by weight is generally chosen. In contrast, in the case of pigmentary dyes which are particularly preferred in terms of lightness but are not readily soluble in water, such as the Pigmosol® dyes mentioned above, suitable dye concentrations in detergents / cleaners are typically Is on the order of several 10 ^-3 to 10 ^-4 % by weight.

Fluorescent Whitening Agent The tablet of the present invention can contain a derivative of diaminostilbene disulfonic acid or an alkali metal salt thereof as a fluorescent whitening agent. Suitable optical brighteners are, for example, salts of 4,4′-bis- (2-anilino-4-morpholino-1,3,5-triazinyl-6-amino) stilbene-2,2′-disulfonic acid Or a compound having the same structure and having a diethanolamino group, a methylamino group, an anilino group or a 2-methoxyethylamino group instead of the morpholino group. Substituted diphenylstyryl type brighteners can also be used, for example, 4,4'-bis- (2-sulfostyryl) diphenyl, 4,4'-bis- (
4-chloro-3-sulfostyryl) diphenyl or 4- (4-chlorostyryl) -4 '-(2
-Sulfostyryl) diphenyl are exemplified. Mixtures of the above whitening agents can also be used.

In the tablet of the present invention, the optical brightener is used in an amount of 0.01% based on the total amount of the tablet.
It can be used at a concentration of 11% by weight, preferably 0.05-0.5% by weight, more preferably 0.1-0.25% by weight.

Perfume According to the present invention, a perfume is added to a detergent tablet to improve the aesthetic effect formed by the product, thereby providing consumers with not only the necessary laundry properties,
Visually and sensorially "typical, non-failure" products can be provided. Suitable perfume oils or fragrances are exemplified by perfuming compounds such as esters, ethers, aldehydes, ketones, alcohols and hydrocarbon-based compounds. Typical ester-based flavoring compounds are benzyl acetate, phenoxyethyl isobutyrate, acetic acid
pt-butylcyclohexyl, linalyl acetate, dimethylbenzylcarbyl acetate,
Phenylethyl acetate, linalyl benzoate, benzyl formate, ethylmethylphenylglycinate, allylcyclohexyl propionate, styralyl propionate and benzyl salicylate. Benzyl ethyl ether is exemplified as an ether-based flavoring compound. As perfuming compounds of the aldehyde, the linear alkanals of C _{8 ~ 18,} citral, citronellal, citronellyloxyacetaldehyde, cyclamen aldehyde, hydroxy citronellal, lilial and bourgeonal, and the like. Suitable ketone-based compounds are ionone, α-isomethylionone, and methylseryl ketone. Examples of the alcohol compound include anethole, citronellol, eugenol, geraniol, linalool, phenylethyl alcohol, terpineol, and the like. Examples of the hydrocarbon compound include terpenes such as limonene and pinene, among others. Preferably, however, a mixture of different fragrances is used, which together produce an attractive aroma. Such perfume oils can include natural flavor mixtures such as those obtained from plant sources, examples of which include pine oil, citrus oil, jasmine oil, patchouli oil, rose oil, ylang ylang oil and the like. . Preferred are sage oil, chamomile oil, clove oil, balsam oil, mint oil, cinnamon oil, lime-blossom oil, juniper berry oil, vetiver oil, olive oil, galvanum oil, labodanum oil, orange brossam oil , Neroli oil, orange peel oil,
Sandalwood oil and the like are exemplified.

The detergent / detergent tablet perfume content of the present invention is usually up to 2% by weight of the total tablet. Perfumes can be directly incorporated into the tablets of the present invention. In another advantageous embodiment, the fragrance is applied to a carrier which enhances the attachment of the fragrance to the laundry, and the slow release of the fragrance ensures long-lasting perfume on the laundry. An example of a suitable carrier material is cyclodextrin, in which case the cyclodextrin / perfume complex can optionally be coated with other auxiliaries.

Enzymes Suitable enzymes are selected from the group consisting of proteolytic enzymes (proteases), lipolytic enzymes (lipases), starch hydrolases (amylases), cellulases and mixtures thereof. Particularly preferred enzymatically active ingredients are those obtained from bacterial or fungal strains, such as Bacill subtilis (Bacill).
us Subtilis), Basillus licheniformis, Streptomyces griseus and the like. Subtilisin-based proteolytic enzymes are preferably used, and Bacillus lentus (Bacill
Us lentus) are particularly preferred. Of particular interest in this connection are enzyme mixtures, such as mixtures of proteolytic enzymes and starch hydrolases, mixtures of proteolytic enzymes and lipolytic enzymes, mixtures of proteolytic enzymes and cellulases, and cellulases. Examples thereof include a mixture of lipolytic enzyme, a mixture of proteolytic enzyme, amylolytic enzyme and lipolytic enzyme, and a mixture of proteolytic enzyme, lipolytic enzyme and cellulase. Particularly preferred is a mixture containing cellulase. In some cases, peroxidases (peroxidases) and oxidases (oxidases) have also proven suitable.

The enzyme can be absorbed by a carrier substance and / or encapsulated by a membrane material, thereby protecting the enzyme from premature degradation. The proportion content of enzymes, enzyme mixtures or enzyme granules may be, for example, about 0.1 to 5% by weight, preferably about 0.1 to 2% by weight, based on the tablet weight.

Soil Release Agent In addition, the detergent / cleaner tablets of the present invention may contain components that facilitate the removal of grease from textiles by washing (so-called soil release agents). This accelerating effect is particularly evident when textiles already containing such an oil-soluble component and already repeatedly washed with the tablets according to the invention become soiled. Suitable anti-redeposition agents include nonionic cellulose ethers such as methylcellulose and methylhydroxypropylcellulose (15-30% by weight of methoxy groups and 1-15% by weight, respectively, based on the amount of nonionic cellulose ether). (Including hydroxypropyl groups), and known phthalic acid and / or terephthalic acid polymers and their derivatives, especially polymers of ethylene terephthalate and / or polyethylene glycol terephthalate and their anionic and / or nonionic modified derivatives. Is exemplified. Of these, the sulphonated derivatives of phthalic acid and terephthalic acid polymers are particularly preferred.

General Tablet Manufacturing Process The detergent / cleaning tablets of the present invention are manufactured by placing the mixture to be tableted into a cavity of a press and compressing it. Tablet manufacturing (hereafter,
It is simply called “tablet”. In the simplest case), the mixture to be compressed is compressed directly (ie, without prior granulation). This so-called direct compression method is simple and cost-effective. This is because no other steps (and thus no additional equipment) are required. However, such advantages are offset by the following disadvantages. For example, a powder mixture to be compressed directly needs sufficient plastic deformation properties and good flow properties. In addition, the powder mixture should not show any tendency for phase separation during storage, transport, filling of dies, and the like. Unfortunately, for many mixtures, these three requirements can only be achieved with significant difficulty. For this reason, the direct compression method, especially for the production of detergent / cleaning tablets, is hardly adopted. That is, the usual method of manufacturing detergent / detergent tablets starts with a fine powder component ("primary particles"), which is conventionally agglomerated or granulated to form larger size secondary particles. I do. The granules or granule mixture obtained are then mixed with the respective powder-form additives and the mixture is compressed.

A preferred detergent / detergent tablet of the present invention is a granular premix comprising at least one surfactant-containing granule and at least one powder-forming component added afterwards (post-added powder-forming component). Obtained by tableting. According to one preferred embodiment of the present invention, the surfactant-containing granules are prepared by standard granulation methods, such as a mixer,
It can be manufactured by bread granulation, fluid bed granulation, extrusion, pelletization or compression. For later detergent / detergent tablets, it is advantageous for the bulk density of the premix to be compressed to approach that of a conventional compressed detergent. Particularly preferably, the bulk density of the premix to be tableted is at least 500 g / l, preferably at least 600 g / l, in particular above 700 g / l. Another advantage can be obtained by using surfactant granules having a relatively narrow particle size distribution. According to one preferred embodiment of the present invention, the particle size of the surfactant-containing granules is between 100 and 4,000 μm, preferably between 100 and 2,000 μm, more preferably between 600 and 1,400 μm.

According to another preferred embodiment of the present invention, the subsequently mixed components include a bleaching agent having such a particle size distribution.

Powdering the Premix According to the present invention, the premix can be "pulverized" with a particulate surface treatment prior to compressing the granular premix to form a detergent / cleaner tablet. . This is advantageous for the quality / physical properties of both the premix (storage, tableting) and the final detergent / detergent tablet. Fine particle powdering agents have been conventionally known, and usually, inorganic salts such as zeolite and silicate are employed. Preferably, however, the premix is pulverized with fine-particle zeolites, preferably faujasite-type zeolites.

Faujasite-type zeolite As used herein, the term “faujasite-type zeolite” means all three zeolites that constitute the faujasite subgroup of zeolite structure group 4 [Don
ald W. Breck: "Zeolite Molecular Sieves", Jhon Wieley & Sons, New York, London, Sydney, Toronto, 1974, p. 92]. Thus, according to the invention, in addition to zeolite X, zeolite Y and faujasite and mixtures of these compounds can also be used, but zeolite X alone is preferred. The co-crystallized mixture of the hojasite-type zeolite and another zeolite does not necessarily belong to the zeolite structure group 4, but can be used in the present invention. In this case, it is advantageous for at least 50% of the zeolite component to consist of faujasite-type zeolites.

According to the invention, preferably, the detergent / detergent tablet is composed of a granular premix, which comprises a granulate component, a post-mix powder forming component (post-adding powder forming component) and Comprising. In this case, the post-mixed powder forming component is a faujasite-type zeolite having a particle size of less than 100 μm, preferably less than 10 μm, and especially less than 5 μm.
It is less than μm and the dose is at least 0.2% by weight, preferably at least 0.5% by weight, especially more than 1% by weight, based on the premix to be compressed. Post-processing component (post-added powder forming component) The fine particle post-processing component having the above-mentioned particle size can be dry-mixed with a premix to be tableted. However, it is also possible and preferred that the component can be deposited on the surface of relatively coarse particles by adding a small amount of a liquid component. Such pulverization methods are described in numerous documents and are well known to those skilled in the art.
A liquid component suitable as an adhesion promoter for the powdering agent is, for example, a surfactant such as a nonionic surfactant or an aqueous solution thereof. According to a preferred embodiment of the present invention, as a liquid component for promoting adhesion between the powdering agent and the coarse particle component,
Perfumes can be used.

Method of Making Tablets To make the tablets of the present invention, the premix is compressed between two punches in a die to form a solid compact. Hereinafter, this step is referred to as a tableting step for simplicity, and comprises four steps (weighing, compression (elastic deformation), plastic deformation, and ejection).

The tableting process can be carried out on a commercial tableting press, which is generally equipped with single or double punches. In the latter case, not only is the upper punch used to form the compression force, but the lower punch also moves toward the upper punch during the tableting process, and the upper punch compresses downward. For small-scale production, an eccentric press for tablets is preferably employed. In this press, a punch is fixed to an eccentric disk, which is mounted around a shaft that rotates at a predetermined speed. Such a punch movement is comparable to the operation of a normal four-stroke engine.
Tableting can be performed by upper punch and lower punch, but some punches
It can be fixed to a single eccentric disk, in which case the number of die holes is correspondingly increased.
Depending on the type of eccentric press, the throughput varies from several hundred up to 3,000 tablets / hour.

For large-scale production, a rotary tablet press is generally employed. In a rotary tablet press, a relatively large number of dies are arranged on a circular die table. The number of dies varies between 6 and 55, depending on the model, but more dies are commercially available. The upper punch and the lower punch communicate with each die on the die table, and the tablet compression force is effectively formed by both the punches as well as the upper punch or the lower punch as described above. The die table and punch move about a common vertical axis, and the punch is carried by curved guide rails to the location of the filling, compression, plastic deformation and discharge process. In locations where a long up / down movement of the punch is required (
Such curved guide rails are supported by additional depressing members, pull-down rails and discharge channels. The die is filled from a fixed feeding device (so-called filling shoe), which is connected to a storage container for the premix. The compression force on the premix can be adjusted independently by the components for the upper and lower punches, and the compression force is formed by rotation of the shaft head of the punch past an adjustable pressure roller.

If an increase in throughput is required, a rotary press with two or more filling shoes can be used. These filling shoes suffice in a circle that moves only half to make one tablet. When producing a two-layer or multi-layer tablet, the first layer, formed by arranging several filling shoes in series and pressing lightly,
It is not discharged before further filling. With certain suitable process controls, inlay tablets having a structure similar to the laminated tablet and onion skin can be formed in this way. In the case of an inlay (bullseye) tablet, the top surface of the core, the core layer, remains visible because it is not covered. Rotary tablet presses can also be equipped with single or multiple punches, so that, for example, an outer circle of 50 holes and an inner circle of 35 holes can be used simultaneously for tableting. Modern rotary tablet presses have a throughput of over one million tablets per hour.

A tableting machine suitable for the present invention can be obtained, for example, from the following production companies. Apparatebau Holzwarth GbR, Asperg, Wihelm Fette GmbH, Schwarzenb
ec, Hofer GmbH, Weil, KIKIAN, Cologne, KOMAGE, Kell am See, KORSCH Press
en GmbH, Berlin, Mapag Maschinenbau AG, Bern (Switzerland) and Couroy N
.V. Halle (BE / LU). An example of a particularly suitable tablet press is the HPF 630 hydraulic double press (LA
EIS, D).

Tablet Form and Dimension The tablet of the present invention can be manufactured in a predetermined form and a predetermined size.
It is always composed of several phases, ie layers, inclusions or cores and rings.
Suitable forms can be virtually any form that can be easily handled, for example, slabs, bars, cubes, blocks, corresponding forms with flat sides, especially circular cross sections or lengths It is a cylindrical form having a circular cross section. This last embodiment encompasses from tablet form to compact cylindrical form with height / diameter ratios exceeding one.

In addition, it is possible to form a divided press body composed of components separated from each other,
Each element corresponds to a predetermined dose of a detergent / cleaner. However, it is possible to form a press body in which several such elements are combined in a single press body, and in this case, a smaller split unit is used, particularly from a predetermined weak spot setting portion,
Can be easily separated. In a standard horizontal washing machine in Europe, in order to use laundry detergent, it is advantageous to manufacture the above-mentioned split press body as a tablet in a cylindrical shape or a block shape, and preferably, The diameter / height ratio is from about 0.5: 2 to about 2: 0.5. Commercially available hydraulic presses, eccentric presses and rotary presses are particularly suitable for the production of such press bodies.

Another aspect of the three-dimensional form of the tablet of the present invention is that its dimensions are adapted to the detergent chamber of a commercial household washing machine, whereby the tablet can be directly
That is, the tablet can dissolve during the water dispensing operation without the use of a weighing tool and can be weighed into the detergent dispensing chamber. However, it is, of course, possible to use a laundry detergent tablet using a measuring instrument, and this embodiment is suitable for the present invention.

Other suitable multi-phase tablets that can be produced are tablets having a sheet-like or rod-like structure having alternating long and thin sections and thin and short sections. Each part breaks at a predetermined break point (thin and short part) and is cut off from the "rod",
Can be introduced into the machine. Also, the principle of this "bar" of laundry detergent can be embodied in other geometries, for example, a vertical triangle which joins each other only at one of their longitudinal sides. In this case, for visual reasons, the parts are preferably interconnected as one phase, while the vertices form the base of the triangle by forming the second phase. In this embodiment, two different colors are particularly attractive.

After breaking compression of the cylindrical tablets , the detergent tablets show a high stability. The fracture resistance of the cylindrical tablet can be determined from the diametral fracture stress. This is given by the equation: σ = 2P / πD
It can be calculated by t. In the formula, σ is the fracture stress in the diameter direction (DFS, Pa), P is the force (N) at which the tablet is broken by compression, D is the diameter of the tablet (m), and t is its height It is.

Example Surfactant granules were mixed with other additives and the resulting mixture was tableted with an eccentric tableting press to produce a bleach-containing detergent / detergent tablet. The bleach (sodium perborate monohydrate) was mixed with the added ingredients, but the bleach has a different particle size distribution depending on the type of tablet. The composition of the surfactant is shown in Table 1 below, while the composition of the premix to be tableted (and therefore the composition of the tablet) is shown in Table 2. Table 3 shows the particle size distribution of sodium perborate monohydrate used for various tablets.

[Table 1]: Surfactant granules [% by weight]

[Table 2]: Premix [% by weight] ^* Compressed cellulose (particle size: 90% by weight> 400 μm)

[Table 3]: Particle size distribution of sodium perborate monohydrate [% by weight]

Hardness Test, Disintegration Test and Detergent Injection (Distribution) Test Tablet hardness was measured by deforming the tablet until it disintegrated. In addition, the force measured the maximum force which the tablet can endure in addition to the side surface of the tablet. For the tablet disintegration test, the tablets were placed in a glass beaker filled with water (temperature 30 ° C., 600 ml) and the time required for the tablets to completely disintegrate was measured. The two tablets were placed in the detergent dispense room of a commercial electric washing machine and the washing program was started. At the end of the detergent charging stage, the detergent charging chamber was removed from the electric washing machine and evaluated visually. If the presence of the residue was visually apparent in the detergent dosing chamber, such a tablet was determined to be in a dispensable (distributable) state.

[0093] Each premix was tableted with an eccentric tableting press to produce a series of tablets. Two types of tablets having different hardnesses were produced by changing the compression pressure. The results are shown in Table 4 below.

[Table 4]: Physical property data of detergent tablets As is clear from the above results, the tablets E1 and E1 ′ of the present invention have improved detergent / detergent performance against stains (eggs, blood, cocoa) which can be removed by enzymes, in addition to excellent physical properties. Indicated.

──────────────────────────────────────────────────続 き Continuing on the front page (72) Christian Brock, Germany Day 50733 Cologne, Wardburgplatz 12 (72) Inventor Monica Becker Germany-Day 42799 Reichlingen, Im Rotfeld No. 14 (72) Heinke Jevens Federal Republic of Germany Day 40589 Düsseldorf, Ittstraße No. 35 (72) Inventor Hans-Friedrich Kurse Federal Republic of Germany Day 41352 Korschen Bloich, Am Hallenbad 44 (72) Inventor Andreas Rietzmann Federal Republic of Germany Day 44805 Bochum, Am Nordbad 88 (72) Inventor Antoni Machin Spain, A-08013 Barcelona No. 279, Avenida Diagonal, Tercelo Primera (72) Inventor Fret Shamville Day 40789 Monheim, Niederstrasse 96, Germany F-term (reference) 4H003 AB03 AB19 AB27 AC08 BA17 CA08 DA01 DA19 EA15 EA16 EA28 EB28 EB16 EB24 EB30 EB42 EC01 ED02 EE05 FA32 FA38

Claims (15)

[Claims] 1. A compressed granular detergent / detergent detergent / detergent tablet comprising a bleach, a builder and optionally other detergent / detergent components, wherein the bleach has an average particle size greater than 0.4 mm. A tablet having a diameter. 2. The tablet according to claim 1, wherein the bleaching agent is substantially free of particles having a particle size of less than 0.2 mm. 3. The bleaching agent according to claim 1, wherein the bleaching agent comprises particles having a particle size of less than 0.4 mm in an amount of less than 30% by weight, preferably less than 20% by weight, more preferably less than 10% by weight. Tablet. 4. The bleaching agent comprises particles having a particle size of more than 0.8 mm in an amount of more than 10% by weight, preferably more than 20% by weight, more preferably more than 30% by weight. The tablet according to any one of 1 to 3. 5. The tablet according to claim 1, wherein the bleaching agent is substantially free of particles having a particle size of more than 1.6 mm. 6. The tablet according to claim 1, wherein the bleaching agent is sodium perborate, particularly sodium perborate monohydrate. 7. The tablet according to claim 1, further comprising one or more bleach activators. 8. The tablet according to any one of claims 1 to 7, further comprising one or more surfactants. 9. The method according to claim 1, which is obtained by tableting a granular premix composed of at least one surfactant-containing granule and at least one powder-forming component to be added later. Tablet. 10. The tablet according to claim 9, wherein the surfactant-containing granules are obtained by standard granulation methods, such as mixer, pan granulation, fluid bed granulation, extrusion, pelletization or compression. 11. The surfactant-containing granules have a particle size of 100 to 4,000 μm, preferably 1 to 4,000 μm.
The tablet according to claim 9 or 10, which has a size of from 00 to 2,000 µm, more preferably from 600 to 1,400 µm. 12. The tablet according to claim 9, wherein the powder-forming component added later contains a bleaching agent. 13. The method according to claim 9, wherein the bulk density of the premix is at least 500 g / l, preferably at least 600 g / l, more preferably at least 700 g / l. Tablet. 14. A disintegrant, preferably a cellulosic disintegrant, more preferably a disintegrant in granular, cogranular or compressed form (particularly cellulosic disintegrant)
14. The tablet according to any one of claims 1 to 13, comprising 0.5 to 10% by weight, preferably 3 to 7% by weight, more preferably 4 to 6% by weight, based on the tablet weight. 15. An enzyme, a pH regulator, a fragrance, a fragrance carrier, a fluorescent agent, a dye, a foam control agent, a silicone oil, a redeposition inhibitor, a fluorescent brightener, a discoloration inhibitor, a dye migration inhibitor, and an anticorrosion. The tablet according to any one of claims 1 to 14, comprising one or more substances selected from the group consisting of agents.