JPH07286199A - Method for producing tablet detergent composition - Google Patents

Abstract

PURPOSE:To obtain a tablet detergent having a sufficient tablet strength for transfer and transportation and capable of being rapidly dissolved in water to express a washing force, when put in the water. CONSTITUTION:The method for producing the tablet detergent composition comprises homogeneously mixing an anionic surfactant and/or a nonionic surfactant in an amount of 5-50wt.% based on the final composition with other detergent components and >=20wt.% of water, granulating the mixture into (A) surfactant-containing granules, mixing (A) the obtained surfactant-containing granules with (B) a granular dissolution-accelerating agent having a solubility of >=20g/100ml in water at 0 deg.C and having an average maximum granule diameter of >=300mum, and subsequently tableting the mixture.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a tablet type detergent composition having excellent tableting strength and solubility.

[0002]

2. Description of the Related Art Conventional laundry detergents contain a bulking agent having a bulk density of 0.3 g / min. It was manufactured as a bead-shaped hollow particle of about cc. However, since such a detergent has a low specific gravity and a low concentration of an activator, transportation costs are high, and a considerable space is required for storage and display. Further, even in a general household, there are inconveniences such as a place to put it in place and difficulty in weighing. Therefore, recently, a high bulk density granular detergent that can be washed with a small amount of detergent has been put on the market.

[0003] In order to further improve the convenience, the development of a tablet detergent has been attempted recently. However, while tablet detergents are simple and easy to use,
There is a difficult technical problem that a high tablet strength for maintaining the shape in the transportation process and a rapid solubility in water must be compatible. Usually, when the tablet strength is increased by increasing the tableting pressure with the same composition, the solubility is deteriorated, and it has been difficult to make these two properties compatible.

Tablets used in other fields such as pharmaceuticals and foods are also required to have disintegrability in water.
In tablets in these fields, in general, in addition to the main component, succinic acid and sodium carbonate or sodium hydrogen carbonate are mixed in a dry state to form tablets, and the acid and carbonate react when contacted with water. A method of improving the disintegration property and promoting the dissolution of the main component by causing carbon dioxide to be generated.

However, in a tablet detergent, if a surfactant is blended with the foaming component as the main active component, the mold adheres to the product during the production, resulting in a marked deterioration of the productivity and the tablet disintegration. There was a problem that the sex itself was insufficient. Furthermore, during storage of the tablet detergent, it absorbs the water contained in it and the water in the air, and the acid-alkali reaction gradually occurs to generate carbon dioxide, so the packaging container expands during storage. Or
There is a drawback that the tablet expands and deforms, and when the tablet detergent is put into water after storage, the disintegration property is significantly deteriorated.

Further, the present applicant has previously proposed to improve the disintegration property of a tablet detergent in water and the mold releasability at the time of production by adding a poorly water-soluble carboxymethylcellulose powder as a disintegrating agent (special feature: Kaihei 2-3116
No. 00).

More recently, a tablet detergent having a good solubility without using a disintegrant has been proposed by using a nonionic surfactant as a main surfactant, and combining it with an A-type zeolite and a porous oil absorbing carrier. (JP-A-4-30
No. 6299, No. 5-65500). However, the detergent of this composition is apt to cause capping (a phenomenon in which the upper surface or the lower surface of the tablet peels off like a hat) during tablet molding, and even if the molding pressure is increased, a tablet having sufficient strength to withstand transportation and transportation is obtained. It has a problem that it is not possible. Furthermore, the solubility is also insufficient at low temperatures that assume the use of tap water in winter.

[0008]

The present invention overcomes these drawbacks of the prior art and produces a tablet detergent having a high tablet strength capable of withstanding production and transportation and having an easy solubility in water. The purpose is to

[0009]

The method for producing a tablet detergent composition according to the present invention comprises the steps of adding an anionic surfactant and / or a nonionic surfactant in an amount of 5 to 50% by weight in the final composition. After being uniformly mixed with a detergent component in a state of water content of 20% by weight or more and granulated to obtain (A) a surfactant-containing granulated product, the solubility in water at 0 ° C. is 20
It is characterized by mixing (B) the granular dissolution promoter having an average maximum particle size of 300 μm or more with g / 100 ml and the (A) surfactant-containing granulated product to form tablets.

[0010]

BEST MODE FOR CARRYING OUT THE INVENTION In the present invention, a tablet detergent composition is prepared by tableting the (A) component-containing granule containing a surfactant and (B) the granular dissolution accelerator. The surfactant to be added to the component (A) is an anionic surfactant and / or
Alternatively, a nonionic surfactant is used. Examples of the anionic surfactant include sulfonates, sulfates, phosphates and carboxylates, and the following can be exemplified.

1) a linear alkylbenzene sulfonate having an alkyl group having an average carbon number of 8 to 16; 2) an α-olefin sulfonate having an average carbon number of 10 to 20; and 3) a fatty acid residue having 8 to 22 carbon atoms. Sulfonates of fatty acid lower alkyl esters of

4) Alkyl sulphate having an average carbon number of 10 to 20 5) Ethylene oxide having an average of 10 to 20 linear or branched alkyl or alkenyl groups and an average of 0.5 to 8 mol Alkyl ether sulfate, alkenyl ether sulfate, or alkyl or alkenyl ether carboxylate having added

6) Saturated or unsaturated fatty acid salt having an average carbon number of 10 to 22. Alkali metal salts such as sodium and potassium are usually suitable as counterions in these anionic surfactants.

The following are examples of nonionic surfactants. 1) An EO addition type nonionic surfactant (alkyl ether ethoxylate) obtained by adding 10 to 25 mol of ethylene oxide (EO) on average to a primary or secondary alcohol having 8 to 18 carbon atoms. 2) E obtained by adding an average of 10 to 25 mol of ethylene oxide (EO) and 3 to 10 mol of propylene oxide (PO) to a primary or secondary alcohol having 8 to 18 carbon atoms.
O-PO addition type nonionic surfactant. 3) Fatty acid polyoxyethylene alkyl ether represented by Chemical formula 1

[0015]

[Chemical 1] n: The number of moles of ethylene oxide added, which is 10 to 10 on average
Number of 30 R ₃ : alkyl group having 1 to 5 carbon atoms)

This nonionic surfactant is an alkyl ether of an ethylene oxide adduct of a fatty acid in which ethylene oxide is added between ester bonds. The ethylene ether is added to the fatty acid by a conventional method, and then alkyl ether is formed. The presence of a catalyst composed of magnesium oxide to which one or more metal ions selected from, for example, trivalent aluminum ions, gallium ions, indium ions, thallium ions, and divalent manganese ions are added. It can also be produced by a one-step method in which a fatty acid alkyl ester and ethylene oxide are reacted below (JP-A-4-279552).

4) A sugar ester nonionic surfactant comprising an ester of a fatty acid having 6 to 18 carbon atoms and a monosaccharide having 5 to 6 carbon atoms or a monoalkyl ether thereof. 5) A sugar alkyl ether-based nonionic surfactant represented by Chemical formula 2.

[0018]

Embedded image R ₁ O (CH ₂ CH ₂ O) n (Z) x (R ₁ : an alkyl group having 8 to 18 carbon atoms n: 0 to 12 Z: a sugar residue having 5 to 6 carbon atoms x: 1 2-10)

6) Alkanolamides of fatty acids having 8 to 18 carbon atoms. 7) Alkyl (C8-18) dimethylamine oxide. In the present invention, only the anionic surfactant may be used as the surfactant blended in the component (A), only the nonionic surfactant may be used, and the anionic surfactant and the nonionic surfactant may be combined. You may use together. Furthermore, in each of the anionic surfactant and the nonionic surfactant, one type may be used alone, or two or more types may be used in combination. The tablet detergent contains 5 to 50% by weight, preferably 10 to 40% by weight, of an anionic surfactant and a nonionic surfactant in total. If the blending amount is less than 5% by weight, sufficient strength cannot be obtained during tablet molding. On the other hand, if it exceeds 50% by weight, the amount of other components such as builders to be blended is reduced, which is not preferable.

In the present invention, the surfactant and the other detergent components are uniformly mixed in a state where the water content is 20% by weight or more, and granulated to obtain a surfactant-containing granulated product of the component (A). . If the water content during this mixing is less than 20% by weight, sufficient tablet strength cannot be obtained. Further, the water content at the time of this mixing is preferably 20 to 60% by weight.

This mixing and granulation can be carried out, for example, as follows. A method in which water content of a surfactant and other detergent components is adjusted and uniformly mixed to form a paste, which is extruded, further dried, and optionally pulverized. A method in which a surfactant and other detergent components are adjusted in water content and uniformly mixed to form a slurry, which is then spray-dried. The average particle size of the surfactant-containing granulated product thus obtained is preferably 150 to 2000 μm, and more preferably 300 to 1000 μm.

Further, as the other detergent component mixed with the surfactant in the production of the component (A), a powder raw material containing a detergent main component is mainly used. For example, sodium tripolyphosphate or sodium pyrophosphate is used. Inorganic builder; aluminosilicate (zeolite), sodium citrate, sodium ethylenediaminetetraacetate, nitrilotriacetate, sodium polyacrylate, sodium acrylate-sodium maleate anhydride copolymer, polyacetal carboxylate, etc. Builders: Alkali builders such as sodium carbonate, potassium carbonate, silicates; Sulfites, sulfates; Recontamination inhibitors such as polyethylene glycols; Enzymes such as proteases, lipases, cellulases, amylases; Quaternary ammonium salts, bentonas Flexible imparting agents such as preparative; bleaches, can be used fluorescent agents, perfumes, dyes and the like.

A part of these detergent components (for example, enzyme, bleaching agent, etc.) can be powder-mixed at the time of tableting. In the present invention, the surfactant-containing granules of component (A) and the granular dissolution accelerator of component (B) are then tableted together with other powdery or granular detergent components such as enzymes, if necessary. Use tablet detergent.

The granular dissolution accelerator as the component (B) is required to have a solubility in water at 0 ° C. of 20 g / 100 ml or more, preferably 30 g / 100 ml or more. If the solubility at 0 ° C. is less than 20 g / 100 ml, the effect of improving the solubility cannot be obtained.

Further, the granular dissolution accelerator of the component (B) is
The average maximum particle size is 300 μm or more, preferably 50
0 μm or more, more preferably 1000 to 1500 μm
Is. If the average maximum particle size is less than 300 μm, a sufficient dissolution promoting effect cannot be exhibited.

The granular dissolution accelerator as the component (B) is roughly classified into spherical particles prepared by rolling granulation or fluidized granulation, and rod-shaped particles produced by extrusion granulation. . In the case of spherical particles, it means a general average particle diameter, and as described above, it is 300 μm or more, preferably 500 μm or more.
It is at least μm, more preferably 1000 to 1500 μm. On the other hand, in the case of rod-shaped particles, the average length is 300 μm.
Or more, preferably 500 μm or more, more preferably 1
It is preferably at least 5 mm and at most 5 mm. The diameter of the cross section of the rod-shaped particles is preferably 100 µm or more, more preferably 300 to 1000 µm.

As the granular dissolution accelerator of the component (B),
Inorganic ammonium salts such as potassium carbonate, ammonium sulfate, and ammonium chloride, sodium benzoate, sodium benzenesulfonate, sodium p-toluenesulfonate, sodium xylenesulfonate, sodium chloride, citric acid, D-glucose, urea, and so on. Examples include sucrose.

In the present invention, the granules containing the surfactant (A), the granular dissolution accelerator (B) and other powdery or granular components such as enzymes are compressed to give tablets. Although a tablet detergent can be obtained, it is preferable to preliminarily granulate most of the main ingredients of the detergent together with the surfactant to obtain the surfactant-containing granule of the component (A). By uniformly dispersing the surfactant together with other detergent components into a surfactant granulated product, and then tableting it, a tablet detergent that has both sufficient strength to withstand transport and transportation and practical low temperature solubility is obtained. Easily obtained. Sufficient tablet strength cannot always be obtained by powder-mixing the powdery surfactant, the granular dissolution promoter of the component (B) and the other powder component and tableting.

In particular, in the present invention, the total amount of the surfactant-containing granulated product and the granular dissolution accelerator is 9% of the final tablet detergent, with the final tablet detergent being 100% by weight.
Tableting is preferably performed in an amount of 0% by weight or more.

The tablet detergent composition of the present invention can be easily molded by tableting according to a usual tablet molding method, and has a diameter of about 20 to 60 mm and a thickness of about 5 to 20 m.
In the shape of m, each tablet is formed into a tablet having a weight of about 5 to 60 g. The water content of the powder mixture used for tableting is 2
0 wt% or less is suitable, and 1 to 15 wt% is suitable. If the water content is too low, the solubility will deteriorate, while if the water content is too high, bleeding will occur.

[0031]

According to the present invention, an anion or nonionic surfactant is mixed with other detergent components in a state of water content of 20% by weight or more to prepare surfactant-containing particles, and the particles having specific characteristics are obtained. A tablet detergent that has a tablet strength sufficient for transfer and transportation by mixing powder with a granular dissolution promoter and tableting, and that is capable of quickly dissolving and exhibiting detergency when placed in water is obtained. can get.

[0032]

EXAMPLES The effects of the present invention will be described more specifically below with reference to examples. Prior to this, the evaluation method used in the examples will be described. (1) Method for measuring tablet strength The strength of the tablet detergent prepared in Example was measured when a force was applied in the diameter direction from the side surface of the tablet using a TS-50N type tablet hardness meter manufactured by Okada Seiko Co., Ltd. . The compression end speed of the load cell was set to 20 mm / min. Strength 3.
A tablet strength of 5 kgf / cm ² or more was judged to be sufficient.

(2) Solubility Evaluation Method (Dissolution Time) After the tablet detergent prepared in the example was left indoors for 1 day,
Put in a beaker filled with tap water of 2 liters at 10 ° C, and use a constant speed stirrer at a speed of 250 rpm for 10
Stir for minutes. The residue was filtered, air-dried for 1 day, and then weighed to calculate the dissolved amount. Solubility (%) is the following number 1
It was calculated from the formula.

[0034]

## EQU1 ## Solubility (%) = [1- (weight of residue / weight before addition)] × 100 Solubility of 70% or more was judged to be practically sufficient.

Example A tablet detergent according to the following production method A or production method B was produced, its performance was evaluated, and the results are shown in Table 1. For tableting in both the production methods A and B, 15 g of the powder composition after uniform mixing was placed in a cylinder (die) having an inner diameter of 40 mm,
The tablet detergent having a diameter of 40 mm and a weight of 15 g was obtained by applying a pressure of 0 Kgf / cm ² for 1 minute.

[Production Method A] A detergent paste having a solid content of 70% was prepared by removing the component (B) and the enzyme shown in Tables 1 and 2 below. This detergent paste was extruded through pores having a diameter of 3 mm to make noodles, and dried at 105 ° C. so that the water content was 9%. Then, it was crushed to obtain a surfactant-containing granular material of component (A) having a particle size of 500 μm or less. The component (B) and the enzyme were uniformly mixed with this, and the mixture was tableted and used for the subsequent evaluation. Table 1 shows the evaluation results of tablet strength and solubility.
Shown in 2.

[Production method B] Anion activator / Na carbonate = 9 using the anion activator and carbon Na shown in Table 1 below.
A 40% solids detergent slurry was prepared at a weight ratio of 0/10. This detergent slurry was dried using a countercurrent spray drying tower at a hot air temperature of 250 ° C. so that the water content was 5% to obtain an anion activator-containing spray dried product. Next, amorphous silica as an arbitrary component was uniformly impregnated with the nonionic activator in the component (A), the spray-dried product and the remaining components were uniformly mixed, and then tableted and used for the subsequent evaluation. The evaluation results of tablet strength and solubility are shown in Table 1.

[0038]

[Table 1] Table 1: Composition, production method and evaluation results (part 1) Sample No. 1 2 3 4 5 6 7 8 Composition (wt%): Surfactant AOS-Na 15 15 15 − − − − − AOS- K − − − 15 15 15 − − LAS-Na − − − − − − 15 − LAS-K − − − − − − − 15 Nonion-1 15 15 15 15 − − 15 15 Nonion-2 − − − − − 15 − − − Nonion − 3 − − − − − 15 − − (B) Component Sucrose − − 10 30 − − 10 10 Citric acid monohydrate − − 20 − 30 20 20 20 BS-Na − − − − − 10 − - optional components A-type zeolite 25 25 15 15 15 15 15 15 sulfite Na 2 2 2 2 2 2 2 2 enzyme 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 amorphous silica 5 5 - - - - - - Na-carbonate Bas La emissions scan method BAAAAAAA Rating: molding pressure ^{(Kgf / cm 2) 300 60} 40 40 40 60 40 40 tablet strength ^{(Kgf / cm 2) 1.6 5.3} 5.7 3.8 4.5 4.0 3.8 4.6 solubility (%) 80 40 70 75 80 75 80 85 (1) Sample No. 3 to 8 are Examples, Sample No. 1-2
Is a comparative example (2) Surfactant: AOS-Na: C _{14 to} C ₁₈ sodium α-olefinsulfonate AOS-K: C _{14 to} C ₁₈ potassium α-olefinsulfonate LAS-Na: alkyl straight chain (C ₁₀ -C ₁₄₎ sodium benzenesulfonate LAS-K: a linear alkyl chain (C ₁₀ ~C ₁₄₎ benzenesulfonic acid potassium nonionic -1: fatty ethylene oxide (EO) has an average of 15 moles added between the ester bond of methyl laurate polyoxyethylene ether nonionic -2: C ₁₂ ~C ₁₃ 1 primary alcohol ethylene oxide (EO) EO addition type has an average of 25 moles additional nonionic surfactant nonionic -3: ethylene oxide C ₁₂ -C ₁₃ 1 primary alcohol ( EO) PO addition with an average of 15 moles of EO) and an average of 3 moles of propylene oxide Type nonionic surfactant

Component (B): Sucrose: 1 mm in diameter and 2-3 in length by extrusion granulation.
Powdered granulated sugar molded into mm. Solubility in water at 0 ° C. 66 g / 100 ml. Citric acid monohydrate: granular citric acid 1 with a diameter of 0.5 to 1 mm
Water salt. Solubility in water at 0 ° C. 49 g / 100 ml. BS-Na: granular sodium benzenesulfonate having a diameter of 0.5 to 1 mm. Solubility in water at 0 ℃ 37g / 10
0 ml. Optional components: Enzyme: Savinase 6.0T / Lipolase 100T = 5 /
Mixture of 1 (both are trade names of enzymes manufactured by Novo Co.) Amorphous silica: Tokseal N (manufactured by Tokuyama Soda Co., Ltd.)

[0040]

[Table 2] Table 2: Composition, manufacturing method and evaluation results (Part 2) Sample No. 9 10 11 12 13 Composition (wt%): Surfactant AOS-Na − − − − 5 AOS-K 7.5 − − 20 − LAS-K 7.5 7.5 7.5 − − AS-Na − − 7.5 − − α-SF-Na − 7.5 − − − Nonion-1 − 15 15 − 15 Nonion − 2 15 − − − − (B) Component Sucrose 10 10 − 10-Citric acid monohydrate 20 20 20 20 20 pTS-Na − − 10 − 10 Arbitrary component A type zeolite 15 15 15 15 15 Sulfite Na 2 2 2 2 2 Enzyme 0.5 0.5 0.5 0.5 0.5 Na carbonate Manufacturing method AAAAA evaluation: Molding pressure (Kgf / cm ² ) 60 60 60 40 60 Tablet strength (Kgf / cm ² ) 5.0 4.5 4.6 5.5 4.2 Solubility (%) 80 80 80 70 85 (1) Sample No. 3 to 8 are Examples, Sample No. 1-2
Is a comparative example (2) Surfactant: AOS-Na: C _{14 to} C ₁₈ sodium α-olefinsulfonate AOS-K: C _{14 to} C ₁₈ potassium α-olefinsulfonate LAS-K: alkyl straight chain (C ₁₀ -C ₁₄₎ potassium benzenesulfonate AS-Na: C ₁₂ ~C ₁₅ alkyl sulfate Nariumu _{α-SF-Na: C 12} ~C 18 sodium sulfonate nonionic methyl esters of saturated fatty -1: esters of lauric acid methyl bond Fatty acid polyoxyethylene methyl ether nonion-2 having an average of 15 moles of ethylene oxide (EO) added between the two: C _{12 to} C ₁₃ EO-addition type nonionic surfactant having an average of 25 moles of ethylene oxide (EO) added to the primary alcohol

Component (B): Sucrose: 1 mm in diameter and 2 to 3 in length by extrusion granulation.
Powdered granulated sugar molded into mm. Solubility in water at 0 ° C. 66 g / 100 ml. Citric acid monohydrate: granular citric acid 1 with a diameter of 0.5 to 1 mm
Water salt. Solubility in water at 0 ° C. 49 g / 100 ml. pTS-Na: sodium p-toluenesulfonate having a diameter of 0.1 to 1 mm. Solubility in water at 0 ℃ 35g / 1
00 ml. Optional components: Enzyme: Savinase 6.0T / Lipolase 100T = 5 /
Mixture of 1 (both are trade names of enzymes manufactured by Novo Co.) Amorphous silica: Tokseal N (manufactured by Tokuyama Soda Co., Ltd.)

Claims (1)

[Claims] 1. A final composition is prepared by uniformly mixing 5 to 50% by weight of anionic and / or nonionic surfactants in an amount of 20% by weight or more with other detergent components. After granulating (A) to obtain a surfactant-containing granule, the solubility in water at 0 ° C. is 20 g / 100 ml or more, and the average maximum particle diameter is 300 μm or more (B) a granular dissolution accelerator, and (A) A method for producing a tablet detergent composition, which comprises mixing with a surfactant-containing granulated product and tableting.