JPH0747760B2 - Detergent composition - Google Patents

Description

TECHNICAL FIELD OF THE INVENTION The present invention segregates an inorganic persalt bleach (sodium perborate) and a bleach-sensitive component (bleach-sensitive component).
a novel tablet-like laundry detergent composition which is included together without egation).

BACKGROUND OF THE INVENTION AND PRIOR ART Modern high-performance powder detergents for use in automatic washing machines usually include bleaches consisting of inorganic persalts and certain bleach-sensitive ingredients, especially bleach activators, enzymes and fluorescents. Including whitening agents.

Detergent compositions in tablet form are known to those skilled in the art as described below, and some products are already on the market. Tablets have several advantages over powdered products. That is, it is easy to handle because it does not need to be weighed, it is easy to supply an appropriate amount to the laundry, the ingredients do not irritate the skin and the degree of irritation to sensitive skin is small, and the compactness saves storage space. It also becomes.

However, in compacted tablets the components are more closely assembled than in powders and are prone to adverse interactions and instabilities. It has heretofore been considered impossible to produce high quality tablets containing bleach and a bleach-sensitive ingredient together without any segregation or separation.

For example, US Patent No. 3 953 350 (Kao), Japanese Patent Application No. 60 015 500A (Lion), Japanese Patent Application No. 6
0 135 497A (Lion) and Japanese Patent Application No. 60 135
No. 498A (Lion) discloses a tablet detergent containing a persalt bleach and no bleach sensitive ingredients. In Spain, tablet detergents containing enzymes but no bleach are commercially available. British Patent No. 900 204 (Unilever) discloses a laminated tablet detergent comprising sodium perborate and certain bleach activators, such as sodium acetoxybenzene sulfonate and phthalic anhydride. The example states that tablets containing these ingredients together are unstable unless sequestered in a separating layer.

Surprisingly, in the present invention, the bleach activator is an N-diacylated amine or N, N'-polyacylated amine, especially tetraacetylethylenediamine (TAED),
It was found that isolation as described above was unnecessary. Also,
Other bleach-sensitive ingredients, in particular enzymes and fluorescent agents, can likewise be included without the need for sequestration, which greatly simplifies the production of tablets.

The fully-formulated tablet detergent of the present invention can be easily manufactured by compressing (compacting) a powder.

SUMMARY OF THE INVENTION The present invention provides: (a) sodium perborate; and (b) (b1) one or more N-diacylated amines or
An N, N'-polyacylated amine bleach activator, and optionally one or more types of (b2) enzyme and (b3) a fluorescent agent, one or more types of inorganic persalt bleach sensitive components, and (c) A tablet obtained by compressing a powdered detergent comprising one or more detersive compounds, one or more detergency builders and other optional detergent ingredients, wherein ingredients (a) and (b) are Provide tablets that are not isolated from each other.

The present invention also provides a method for manufacturing a tablet detergent. This manufacturing method comprises the following steps: (i) (a) sodium perborate and (b) (b1) one or more N-diacylated amines or N,
N'-polyacylated amine bleach activator and optionally one or more types of (b2) enzyme and (b3) one or more inorganic persalt bleach sensitive components consisting of a fluorescent agent, and (c) one type Producing a powdered detergent comprising the above-described detersive compound, one or more detergency builders, and other optional detergent ingredients, (iii) compressing the powder to produce ingredients (a) and (b)
Form tablets that are not isolated from each other.

DETAILED DESCRIPTION OF THE INVENTION The tablet detergent of the present invention comprises, as a main component, an inorganic persalt bleach (sodium perborate) and at least one bleach-sensitive component such as an acylated amine bleach activator,
In addition to enzymes, fluorescent agents, surfactants, detergency builders, and optionally other common ingredients. The following is a more detailed description of these various ingredients.

One of the main characteristics of the present invention is sodium perborate (a).
And the one or more bleach-sensitive components (b) are not isolated from each other in the doublet. That is, the ingredients are not randomly separated from one another in specific areas of the tablet, such as a separating layer or insert, but are mixed randomly. This does not mean, however, that these ingredients do not have any form normally used in powder detergents, for example bleach activator in the form of granules, enzymes in the form of granules, marumes or coated marumes. Any protective, coating or dilution means may also be used to obtain these forms. However, in the tablet of the present invention, a means for separating (a) sodium perborate and (b) one or more kinds of bleaching agent sensitive components is used in addition to these means which are generally used in powder detergents. do not do.

In one of the preferred embodiments of the present invention, the tablet of the present invention is substantially homogeneous. That is, it is produced by compressing a single homogenous admixture powder.

However, tablets that include one or more separation layers, inserts or other means for sequestering components other than components (a) and (b) are also within the scope of the invention. In that case,
Ingredients (a) and (b) are mixed at random and distributed in at least one region of the tablet.

Sodium Perborate (a) The inorganic persalt bleach used in the tablet detergent of the present invention is sodium perborate. This material can have a monohydrate, a tetrahydrate, a mixture of the two, a partially dehydrated tetrahydrate, or any other stable commercial form. Sodium perborate monohydrate can have high surface area or low surface area morphology. The content of sodium perborate is preferably 1 to 30% by weight, more preferably 5 to 20% by weight.

Bleach Sensitive Component (b) The tablet of the present invention contains a bleach sensitive component (b1) as one of the main components, and optionally (b2) and (b3).
Of at least one bleach-sensitive component selected from the group of: One or more bleach-sensitive components selected from any one or more of the above groups may be used in any combination.

Bleach activator (b1) The activator that activates the inorganic persalt is an organic compound having one or more reactive acyl residues that induce the formation of peracid. In the presence of peracid, a greater effect is obtained at low wash temperatures, for example around 20-60 ° C, than when using only inorganic persalts.

The bleach activators used in the tablets of the present invention are N-diacylated amines or N, N'-polyacylated amines.
These substances are described in British Patent No. 855 355 and British Patent No. 907.
No. 356 (Unilever). In the case of polyamines, at least one nitrogen atom must carry two acyl groups. The preferred bleach activator for use in the tablets of the present invention is tetraacetylethylenediamine (TAED).

The weight ratio of inorganic persalt (sodium perborate) to bleach activator in the tablets of the present invention may vary from about 30: 1 to about 1: 1, preferably 15: 1 to 2: 1. To do.

TAED is advantageously used in the form of granules with the organic carrier as the carrier. The content of TAED itself in the tablet of the present invention is preferably 1 to 15% by weight, more preferably 2 to 10% by weight.

Enzyme (b2) The tablet detergent of the present invention may optionally use various detergency enzymes well known to those skilled in the art for their ability to decompose and promote the removal of various stains and stains. .

Suitable enzymes include various proteases, cellulases, lipases, amylases, and mixtures of these enzymes formulated to remove various soils and stains from fibers. In the present invention, a proteolytic enzyme (protease) is particularly used.

The preferred protease is a solid catalytically active protein material that typically hydrolyzes proteinaceous stains present as fiber stains. This substance may have any origin such as plants, animals, bacteria or yeast.

Proteases are commercially available in a variety of qualities and origins that are active in the pH range 4-12 and these proteases may be used in the tablet detergent of the present invention. Specific examples of suitable proteases include B. subtilis and B. lichen.
Subtilidines obtained from certain strains of iformis, such as Subtilidine Maxatase (TM) commercially available from Gist-Brocades NV of Delft, The Netherlands, and Alcalase (TM) commercially available from Novo Industri A / S of Copenhagen, Denmark. Can be mentioned.

Particularly suitable for use in the present invention are proteases from Bacillus strains that show maximal activity in the pH range 8-12. It is commercially available, for example, from Novo Industri A / S under the registered trademarks Esperase and Savinase. The production of these and similar enzymes is described in British Patent No. 1 243 785. Other commercially available proteases include Kazu
sase ™ (commercially available from Showa Denko in Japan), Optimase
Trademarks (Miles Kali-Chemie, Hanover, West Germany)
Commercially available) and Superase ™ (commercially available from Pfizer, USA).

Detergent enzymes are usually used in the form of optionally protective coated granules or marumes, the amount of which is about 0.1% by weight to about
It is 3.0% by weight.

Fluorescent agent (b3) In the tablet detergent of the present invention, any fluorescent agent (optical brightener) suitable for use in a powder detergent can be used.

The most commonly used fluorescent agents belong to the diaminostilbene-sulphonic acid derivatives, diarylbirazoline derivatives and bisphenyl-distyryl derivatives.

Examples of the diaminostilbene-sulfonic acid derivative type fluorescent agent include 4,4'-bis- (2-diethanolamino-4-anilino-s-triazin-6-ylamino) stilbene-2: 2'-disulfonic acid disodium salt. , 4,4′−
Bis- (2-morpholino-4-anilino-s-triazin-6-ylamino) stilbene-2: 2'-disodium disodium salt, 4,4'-bis- (2,4-dianilino-s
-Triazin-6-ylamino) stilbene-2: 2'-
Disodium disulfonate 4,4'-bis- (2-anilino-4- (N-methyl-N-2-hydroxyethylamino) -s-triazin-6-ylamino) stilbene-
2,2'-disodium disodium salt, 4,4'-bis- (4
-Phenyl-2,1,3-triazol-2-yl) stilbene-2,2'-disulfonic acid disodium salt, 4,4'-bis (2-anilino-4- (1-methyl-2-hydroxyethylamino) ) -S-Triazin-6-ylamino) stilbene-2,2'-disulfonic acid disodium salt and 2-
(Stillville-4 ″ -naphtho-1 ′, 2 ′, 4,5) -1,2,3
-Triazol-2 "-sodium sulfonate.

A preferred fluorescent agent is Ciba-Geigy AG, Basel, Switzerland.
Tinopal ™ DMS and Tinopal CB available from
It is S. Tinopal DMS is disodium 4,4'-bis- (2-morpholino-4-anilino-s-triazin-6-ylamino) stilbene disulfonate, Tinopal DMS
Pal CBS is disodium 2,2'-bis (phenyl-styryl) disulfonate.

Another fluorescent agent suitable for use in the present invention is 1,3
-Diallyl pyrazoline and 7-alkylaminocoumarins.

The preferred content of the fluorescent agent is 0.02 to 0.8% by weight, more preferably 0.03 to 0.5% by weight.

Surfactant system The total amount of the cleaning agent (surfactant) of the tablet detergent of the present invention is suitably 2 to 50% by weight, preferably 5
Up to 40% by weight.

The tablet detergents of the present invention may include one or more soaps or non-soap anionic, nonionic, cationic, amphoteric or zwitterionic surfactants, or any suitable combination thereof. Suitable detersive compounds are many commercially available and also include, for example, Schwartz, Perry and Berch, "Surface.
-Detailed in literature such as Active Agents and Detergents ", Vol. I and II.

Preferred detersive compounds that can be used are soaps, synthetic non-soap anionic surfactants and nonionic surfactants.

Synthetic anionic surfactants are well known to those skilled in the art. Specific examples thereof include alkyne benzene sulphonates, especially linear sodium alkylbenzenesulfonate alkyl chain length C ₈ -C _15; primary alcohol sodium sulfate of the first and second alkyl sulfates, especially C ₁₂ -C _15; Olefin sulfonates; alkane sulfonates; dialkyl sulfosuccinates; as well as fatty acid ester sulfonates.

Suitable nonionic detersive compounds which can be used include, in particular, compounds having a hydrophobic group and a reactive hydrogen atom, such as aliphatic alcohols, acids, amides or alkylphenols, alkylene oxides, especially ethylene oxide alone or ethylene oxide and The products obtained by reacting with propylene oxide are mentioned.

Specific non-ionic detersive compounds are alkyl (C _6-
C ₂₂₎ phenols - ethylene oxide condensates, the condensation products of linear or branched aliphatic C ₈ -C ₂₀ primary or secondary alcohols with ethylene oxide, and reaction products of ethylene oxide and propylene oxide and ethylenediamine And the products formed by condensation with. Other so-called nonionic detergent compounds include long chain tertiary amine oxides, tertiary phosphine oxides and dialkyl sulfoxides.

Particularly preferred are C ₁₂ -C ₁₅ primary and secondary alcohols was Etokishiren of the first and second alcohol ethoxylates, especially alcohol per mole average 5 to 20 moles of ethylene oxide.

It may be desirable to include one or more fatty acid soaps. Preferred soaps of this type are sodium soaps derived from natural fatty acids such as those derived from coconut oil, beef tallow, sunflower or hydrogenated rapeseed oil.

Detergent compositions suitable for use in automatic washing machines usually include anionic or nonionic surfactants, or combinations thereof in any proportion. Soap may also be included, if desired, in an amount of 0-40% by weight of the composition. In general, compositions of this type can be made into tablets in the process of the invention without problems.

Builder System The tablet detergent of the present invention contains at least one detergency builder. The amount is suitably 5 to 80% by weight, more preferably 20 to 80% by weight.

Particularly preferred are alkali metal phosphates, alkali metal aluminosilicates and combinations thereof.

Preferred alkali metal phosphates are sodium orthophosphate, sodium pyrophosphate and sodium tripolyphosphate. Sodium tripolyphosphate is especially preferred.
This material will normally be included in up to 50% by weight of the composition.

Alkali metal (preferably sodium) aluminosilicates may generally be used in amounts up to 60% by weight of the composition and have the general formula 0.8-1.5 Na ₂ O. It may be crystalline or amorphous having Al ₂ O ₃ .0.8 to ₆ SiO ₂ , or a mixture thereof.

The aluminosilicate must contain some bound water and have a calcium ion exchange capacity of at least 50 mg CaO / g. Preferred sodium aluminosilicates contain from 1.5 to 3.5 SiO ₂ units (in the above formula). Both amorphous and crystalline materials can be readily prepared by the reaction of sodium silicate and sodium aluminate, as widely described in the literature.

Suitable crystalline sodium aluminosilicate ion exchange detergency builders are described, for example, in GB 1 429 143 (Proctor
& Gamble). Preferred sodium aluminosilicates of this type are the well known and commercially available zeolites A and X, and mixtures thereof. Especially preferred is Zeolite 4A.

The tablet detergent of the present invention may also contain other builders if necessary or desired. One of ordinary skill in the art will readily envision suitable organic or inorganic water-soluble or water-insoluble builders. Alkali metal (usually sodium) carbonates can be used as inorganic builders, and nitrilotriacetate, citrate and carboxymethyloxysuccinate can be used as organic builders.

Particularly preferred other builders are polycarboxylate polymers, especially polymers containing acrylate (meth) acrylate and / or maleate units. These polymers also have additional benefits, such as reducing redeposition. Suitably these polymers are used in amounts of 0.5 to 10% by weight, more preferably 1 to 6% by weight. These polymers may have the acid form or the completely or partially neutralized salt form. Preferred polymers are homopolymers and copolymers of acrylic acid. Particularly advantageous are polyacrylates, acrylic acid / maleic acid copolymers, and acrylic phosphinates: acrylic acid / maleic acid copolymers, for example
BASF's Sokalan ™ CP5 is particularly preferred.

Other Ingredients Other ingredients that may optionally be used in the tablet detergent of the present invention include soil redeposition inhibitors such as sodium carboxymethyl cellulose, polyvinyl pyrrolidone and cellulose ethers such as methyl cellulose and ethyl hydroxyethyl cellulose; stabilizers such as ethylene diamine. Tetramethylene phosphonates and diethylenetriamine pentamethylene phosphonates; textile softeners; foam control agents or foam boosters if appropriate; heavy metal ion sequestering agents such as EDTA; perfumes; colorants; and inorganic salts such as sodium sulfate and magnesium sulfate. There is. Sodium sulphate can be used as a filler in the composition of 40% if desired.
It can be used in an amount of up to% by weight. However, sodium sulfate may be present in an amount of less than 10% by weight of the composition, or may not be included at all.

The tablet detergent according to the invention advantageously comprises an antifoaming agent, especially in the case of tablets mainly for use in front-loading automatic drum washing machines. Suitable defoamers are commonly found, for example, in European Patent Application No. 266 863A (Un
granules as described in “Ilever”. Such granular defoamers typically combine a mixture of silicone oil, petroleum jelly, hydrophobic silica, and alkyl phosphate as an antifoam activator into a carbonate-based porous absorbent water-soluble inorganic carrier material. It consists of what is absorbed. The content of the granular defoamer can be up to 5% by weight of the composition.

The tablet detergent of the present invention comprises an alkali metal silicate,
Especially sodium orthosilicate, sodium metasilicate,
Alternatively, and preferably, it may be desirable to also include suitable amounts of neutral or alkaline silicates. The use of this type of alkali metal silicate, for example in an amount of 0.1 to 10% by weight, can be advantageous in preventing corrosion of the metal parts of the washing machine and can also improve the cleaning effect.

Production of Detergent Tablet The detergent composition of the present invention is produced in a tablet shape by compressing powder. As mentioned above, in one of the preferred embodiments of the present invention, the tablet of the present invention is substantially homogeneous. That is, it is formed by compressing a single, substantially homogeneous powder without the addition of inserts, separating layers containing sequestering components, coatings or the like. Therefore, the manufacturing is extremely simplified. However, for example, the starting powder may include inserts or other localized isolation regions that will later remain in the tablet, or two or more powders may be compressed to form separate layers in the final tablet. The case is also included in the scope of the present invention. The only requirement is that components (a) and (b) not be isolated from each other.

The powder itself may be produced by any suitable method, such as mixing, granulating or any combination of these methods, optionally spraying the liquid components. For example, the solid components may be prepared by dry blending, adding water and / or liquid components, granulating the mixture and then drying. Alternatively, an aqueous slurry of detergent ingredients may be spray dried to form granules and then a heat sensitive ingredient such as a bleach or enzyme may be post-added. Again, the liquid component may be sprayed at any stage of the process.

One of the preferred methods of using spray drying involves the following steps: (i) Spray drying the aqueous slurry to include one or more detersive compounds, one or more detergency builders, and a fluorescent agent to be included. Forming a base powder comprising (b3) and other desired ingredients, (ii) adding sodium perborate (a) to the base powder and any N-diacylated or N, N'-polyacylated amine bleach activator (b1) and / or enzyme (b2) are added and optionally other ingredients to form a homogeneous powder, (iii) the powder is compressed To form a tablet.

Modes of Use The tablet detergent of the present invention can be, and preferably is, formulated to be used as a complete heavy-duty detergent composition for textiles. In this way, the consumer does not need to mix and use several tablets having different compositions.

One tablet may contain all of the ingredients in an amount sufficient to provide exactly the amount required for average laundry, but preferably the consumer will choose a dose depending on the size and type of laundry. As can be varied, each tablet contains a submultiple quantity of the composition required for average laundry conditions. For example, the tablet size may be selected such that two tablets provide sufficient composition for a single average wash load. One or more tablets may be added when the amount of washing is particularly heavy or the stains are severe, and only one tablet may be used when the amount of washing is low or the stains are light.

EXAMPLES The present invention will be described in more detail below with reference to non-limiting examples. The parts and percentages used in these examples are parts by weight and percentages by weight. The examples and compositions of the present invention are indicated by numerals, and the comparative examples and compositions are indicated by letters.

Example 1 A phosphor-free detergent base powder containing a fluorescent agent was prepared with the following composition using spray drying followed by spraying with a 3EO nonionic surfactant.

% Linear Alkylbenzene Sulfonate 9.2 C _{12 to} C ₁₅ 7EO Nonionic Surfactant 4.2 C _{13 to} C ₁₅ 3EO Nonionic Surfactant 9.2 Fatty Acid Soap 2.5 Zeolite 4A (anhydride basis) 36.8 Acrylic Acid / Maleic Acid Copolymer (Sokalan * CP5) 6.0 Sodium silicate 0.7 Sodium carboxymethylcellulose 0.8 Fluorescent agent (Tinopal ** DMS and Tinopal ** CBS-X) 0.3 Sodium carbonate 12.9 100% water remaining * Trademark; manufactured by BASF AG, Ludwigshagen, Germany.

** Trademark; Ciba-Gaigy AG, Basel, Switzerland.

Tablets and powders were prepared with the following composition. The enzyme used was granular protease Savinase ™ 6.0T, sodium perborate was a large surface area (5.9m ² / g) monohydrate, TAED
Is granular (83% by weight TAED, 17% by weight inert phosphorus-free carrier). Example 1 Powder based on P tablet powder 85.4 85.4 Enzyme 1.0 1.0 Perborate 10.0 10.0 TAED Granules 3.6 3.6 Tablets were made using an Instron ™ constant speed extensometer with a crosshead speed of 100 mm / min. , 1.5 kN formed by compressing the powder. Each tablet weighed 60 g, had a diameter of 53 mm and a thickness of about 25 mm.

The performance of these tablets and powders of bleach, fluorescers and enzymes can be determined by the composition of the freshly made, harsh conditions (temperature).
The composition after storage for 1 week and the composition after storage for 2 weeks at 37 ° C., relative humidity 70%, unprotected and unpackaged) were compared. This comparison was carried out by washing the selected test cloths in a tergotometer with hard water 1 of 12 ° hardness (France) for 15 minutes at an isothermal temperature of 40 ° C. The tablets were ground before washing and used at a dose of 5 g / l. The powder dose was also 5 g / l.

Table 1 shows the results of the enzyme performance measured with an enzyme-sensitive test cloth (polyester / cotton cloth with casein stains) as the difference in reflectance (ΔR at 460 nm).

Despite being closer to the bleach component, tablets did not undergo enzymatic degradation more than powder.

Table 2 shows the results of the fluorescent agent performance measured using a fluorescent agent-sensitive test cloth as the difference in reflectance (ΔR at 460 nm) in the presence and absence of ultraviolet light.

Again, no significant difference was seen between the tablet and powder.

Table 3 shows the results of the performance of the bleach as measured by the difference in reflectance (ΔR at 460 nm) measured with a test cotton cloth with tea stains.

Surprisingly, the results were consistently better for tablets than for powders of the same composition.

Example 2 A detergent base powder containing phosphate as a builder and a fluorescent agent was prepared with the following composition using spray drying followed by spraying with a 3EO nonionic surfactant.

% Linear alkyl benzene sulfonate 8.3 C _{12 to} C ₁₅ 7EO Nonionic surfactant 5.3 C _{13 to} C ₁₅ 3EO Nonionic surfactant 3.5 Fatty acid soap 0.7 Sodium tripolyphosphate 29.3 Acrylic acid / maleic acid copolymer (Sokalan CP5) 1.2 Silicic acid Sodium 7.0 Carboxymethylcellulose sodium 0.4 EDTA 0.15 Fluorescent agent (Tinopal DMS and Tinopal CBS-X) 0.35 Sodium carbonate 5.9 Sodium sulfate, the remaining tablet of 100% water and powder were prepared in the same manner as in Example 1 with the following composition. The enzymes, sodium perborate mu hydrate and TAED used are the same as in Example 1.

Example 2 Powder based on Q tablet powder 85.4 85.4 Enzyme 1.0 1.0 Perborate 10.0 10.0 TAED granules 3.6 3.6 The bleach, fluorescent and enzyme performance of these tablets and powders was compared in the same way as in Example 1. . The enzyme results are shown in Table 4, the fluorescent agent results are shown in Table 5, and the bleaching agent results are shown in Table 6.
Shown in.

Again, no significant difference was seen between the tablet and powder.

The bleach performance declined with storage as expected, but surprisingly the results were consistently better with the tablets than with the powders.

Examples 3 to 5 The phosphorus-free base powder of Example 1 and three different types of sodium perborate: large surface area (5.9 m ² / g) monohydrate, small surface area (3.2 m ² / g) one. The comparison was repeated with hydrate and tetrahydrate.

Tablets and powders were prepared with the following composition. Examples 3, 4 and 5 are tablets, Examples R, S and T are powders.

Freshly prepared composition, (temperature 37 ° C, relative humidity 70%
In the same manner as in Example 11, the performance comparison of the bleaching agent and the enzyme was performed on the composition after storage for 2 weeks and the composition after storage for 4 weeks. The results are shown in Table 7 (bleaching agent) and Table 8 (enzyme).

Table 7 (bleach) Example Q 4 3 (tablets) 2.3 0.9 R (powder) 1.5 1.1 4 (tablet) 2.0 0.8 S (powder) 2.4 0.5 5 (Tablet) 1.3 1.6 T (powder) 2.3 0.8 Perborate In the presence of the monohydrate, the bleach performance did drop as expected after 4 weeks of storage, although this was not more pronounced for the tablets than for the powder, and surprisingly the perborate In the case of small surface area materials, tablets showed less performance degradation than powders. Tablets showed better results when the perborate was in the tetrahydrate form.

No big difference was seen.

Examples 6-8 The procedure of Examples 3-5 was repeated with a similar series of compositions also containing TAED (83 wt% phosphorus free granules used in Example 1). Tablets and powders were prepared with the following composition.
Examples 6, 7 and 8 are tablets, Examples U, V and W
Is a powder.

As freshly prepared composition as in Example 1, (temperature 37
Composition after storage for 2 weeks at 4 ° C. and 70% relative humidity and 4
The compositions of bleach and enzyme were compared for the compositions after weekly storage. The results are shown in Table 9 (bleach) and Table 10 (enzyme).
Shown in.

No significant difference was found between the tablet and the powder.

No big difference was seen.

Examples 9 and 10 The procedure of Examples 3 and 6 was repeated using the phosphate builder-containing base powder of Example 2 instead of the phosphorus-free base powder of Example 1. Tablets and powders were prepared with the following composition. Examples 9 and 10 are tablets and Examples X and Y are powders. Example 9, X 10, Y- based powder 89.0 85.4 Enzyme 1.0 1.0 Perhosate (monohydrate, high surface area) 10.0 10.0 TEAD Granules-3.6 As freshly prepared composition as in Example 1, ( Temperature 37
Composition after storage for 2 weeks at 4 ° C. and 70% relative humidity and 4
The compositions of bleach and enzyme were compared for the compositions after weekly storage. The results are shown in Table 11 (bleach) and Table 12 (enzyme).
Shown in.

After storage for 4 weeks, tablets showed better results than powders of the same composition.

No big difference was seen.

Example 11 A bleaching agent composed of sodium perborate tetrahydrate with phosphate as a builder and a proteolytic enzyme (Savinase)
And a powder detergent containing a fluorescer and the following composition were prepared using spray drying and post addition.

% Linear alkyl benzene sulfonate 18.0 C _{12 to} C ₁₅ 7 EO Nonionic surfactant 8.0 Fatty acid soap 2.0 Sodium tripolyphosphate 30.0 Acrylic acid / maleic acid copolymer (Sokalan CP5) 1.5 Alkaline sodium silicate 10.0 Carboxymethylcellulose sodium 0.5 EDTA 0.25 Fluorescent agent: Tinopal DMS 0.13 Tinopal CBS-X 0.08 Sodium sulphate 3.6 Sodium perborate tetrahydrate 10.0 Enzyme (Savinase 6CM) 0.75 Granular defoamer 3.0 Fragrance 0.22 Moisture, 100% salt remaining Powder has a bulk density of 400-425g It was / l. This powder was compressed to about half the volume on a pilot-scale tablet press to form tablets weighing 32 g, diameter 50 mm, thickness 23 mm.

This tablet showed effective washing and washing performance in the washing machine. Appropriate doses were 2 tablets for soft water and 3 tablets for hard water.

Example 12 A powdered detergent comprising phosphate builder and sodium perborate tetrahydrate bleach together with TAED granules, a proteolytic enzyme (Savinase) and a fluorescent agent, with the following composition, spray dried and Produced with the addition and then compressed as in Example 11 to form tablets.

% Linear alkyl benzene sulfonate 18.0 C _{12 to} C ₁₅ 7 EO Nonionic surfactant 8.0 Fatty acid soap 2.0 Sodium tripolyphosphate 30.0 Acrylic acid / maleic acid copolymer (Sokalan CP5) 1.5 Alkaline sodium silicate 10.0 Carboxymethylcellulose sodium 0.5 EDTA 0.25 Fluorescent agent: Tinopal DMS 0.13 Tinopal CBS-X 0.08 Sodium sulphate 1.3 Sodium perborate tetrahydrate 10.0 TAED Granules (83% by weight active ingredient) 2.4 Enzyme (Savinase 6CM) 0.75 Granular defoamer 3.0 Fragrance 0.22 Moisture, salt 100% The rest of the tablets showed effective laundering performance when used at a dose of 2-3 tablets per wash.

Example 13 A bleach containing phosphate as a builder and sodium perborate monohydrate was used as TAED, a proteolytic enzyme (Savina
se) and a more bleaching powder detergent with a fluorescer, with the following composition, using spray drying and post-addition.

% Linear alkylbenzene sulfonate 18.0 C _{12 to} C ₁₅ 7 EO Nonionic surfactant 8.0 Fatty acid soap 2.0 Sodium tripolyphosphate 30.0 Acrylic acid / maleic acid copolymer (Sokalan * CP5) 1.5 Alkaline sodium silicate 10.0 Carboxymethylcellulose sodium 0.5 EDTA 0.25 Fluorescent agent : Tinopal DMS 0.13 Tinopal CBS-X 0.08 Salt 4.24 Water 8.0 Sodium perborate monohydrate 10.0 TAED 3.33 Enzyme (Savinase 6CM) 0.75 Granular defoamer 3.0 Fragrance 0.22 Compress this powder as in Example 11 , Each weight is 26
~ 28g, diameter 40mm, thickness 26mm tablets were formed.
The tablets showed effective laundering performance when used at a dose of 2-3 tablets per wash.

Examples 14 and 15 A phosphorus-free powder detergent containing a bleach consisting of sodium perborate monohydrate with TAED, a proteolytic enzyme (Savinase) and a fluorescent agent, with the composition below, using spray drying and post-addition. Manufactured. This powder was compressed by the method of the present invention to 40
Suitable for forming g tablets.

1 4 15 Linear alkyl benzene sulfonate 18.0 6.0 C _{12 to} C ₁₅ 7EO Nonionic surfactant 3.0 4.5 C _{13 to} C ₁₅ 3EO Nonionic surfactant 5.0 4.0 Fatty acid soap 2.0 − Zeolite 4A (anhydrous base) 30.0 37.0 Acrylic acid / Maleic acid copolymer (Sokalan CP5) 4.0 5.0 Carboxymethylcellulose sodium 0.5 0.5 Fluorescent agent: Tinopal DMS-X 0.13 0.13 Tinopal CBS-X 0.08 0.07 Sodium carbonate 9.0 14.9 Sodium perborate monohydrate 10.0 7.5 TAED granules (83%) 4.5 4.5 Enzyme (Savinase 6.0T) 1.0 1.0 Granular defoamer 3.0 1.5 Fragrance 0.4 0.4 Water and trace components 100.0% Remainder

─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. ⁶ Identification code Internal reference number FI Technical display location C11D 3/42 11/00 (72) Inventor Alan Jyon Fry South Wilal El, UK・ 65/5 Day Elle, Ellesmere Port, Winch Esther Avenue 35 (72) Inventor Geoffrey Newbold England, Merseyside El 63 9 Els, Willal, Bebington, Corey Way 53 (72) Inventor Jionathan Osler United Kingdom, Merseyside L 42/5 LH, Birkenhead, Hier Tranny, Hampden Road 29 (56) References 57-142910 (JP, A)

Claims (5)

[Claims] 1. (a) sodium perborate, and (b) (b1) one or more N-diacylated amines or
An N, N'-polyacylated amine bleach activator, and optionally one or more types of (b2) enzyme and (b3) a fluorescent agent, one or more types of inorganic persalt bleach sensitive components, and (c) Ingredients (a) and (b) are not isolated from each other and are formed by compressing a powdered detergent containing one or more detersive compounds, one or more detergency builders, and other optional detergent ingredients. Laundry detergent tablet. 2. The detergent tablet according to claim 1, which contains tetraacetylethylenediamine as the bleach activator (b1). 3. The detergent tablet according to claim 1, which is substantially homogeneous. 4. (i) (a) sodium perborate and (b) (b1) one or more N-diacylated amines or
An N, N'-polyacylated amine bleach activator, and optionally one or more types of (b2) enzyme and (b3) a fluorescent agent, one or more types of inorganic persalt bleach sensitive components, and (c) Producing a powder detergent comprising one or more detersive compounds, one or more detergency builders and other optional detergent ingredients, (ii) compressing the powder to produce ingredients (a) and (b) ) Forming a tablet which is not isolated from each other. 5. (i) spray drying the aqueous slurry to give 1
Forming a base powder comprising one or more kinds of detersive compounds, one or more kinds of detergency builders, a fluorescent agent (b3) to be contained, and other desired components, (ii) , Sodium perborate (a) and any N-diacylated or N, N'-polyacylated acyl bleach activator (b1) and / or enzyme (b2) to be included, if desired The method of claim 4 including the step of optionally adding other ingredients to form a homogeneous powder, and (iii) compressing the powder to form a tablet.