JPH06128595A - Production of high-bulk-density granular detergent - Google Patents

Abstract

PURPOSE:To produce a detergent excellent in free-flowability and contg. a surfactant in a high concn. without requiring a cooling step, an aging step, etc., by using a hardly degrgadable surfactant salt as the starting material and compounding most or the whole of the surfactant into the detergent by a non-spray-drying method. CONSTITUTION:20-55wt.% thick surfactant paste contg. at least 60wt.% surfactant including at least one anionic surfactant, 20-40wt.% alkaline builder contg. at least either potassium carbonate or hydrogencarbonate, and spray-dried zeolite-contg. particles in an amt. of 5-40wt.% in terms of zeolite are mixed, kneaded, and powdered to give the detergent.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a high bulk density granular detergent containing a surfactant in a high concentration and having a high free flowability.

[0002]

2. Description of the Related Art Conventional laundry detergents contain a bulking agent having a bulk density of 0.1% by adding an extender (usually Glauber's salt) that hardly contributes to the cleaning performance to the composition and spray-drying it.
It was produced as bead-shaped hollow particles of about 3 g / cc.

However, since such a detergent has a low specific gravity and a low concentration of an activator, it is costly to transport and requires a considerable space for storage and display. It was difficult to weigh. Therefore, recently, a method for producing a high bulk density granular detergent which can be washed with a small amount of detergent has been proposed and put on the market. As a method for producing a high-bulk density granular detergent, the following techniques have been conventionally known, centering around the method for producing a laundry detergent, but all have drawbacks.

1) Japanese Unexamined Patent Publication (Kokai) No. 52-30962: A fatty acid having a melting point or higher is neutralized with water-containing powdery sodium carbonate to produce a powdery heavy detergent. <Disadvantage> Heating is required and the solubility of the obtained detergent is insufficient.

2) US Pat. No. 3,434,974: A method of neutralizing alkylbenzene sulfonic acid with sodium hydrogen carbonate, sodium tripolyphosphate and the like. <Disadvantage> Since the surfactant is treated from the acid state, deterioration of the acid with time becomes a problem, and sodium hydrogen carbonate needs to be used, and the product contains a relatively large amount of water.

3) JP-A-60-72999: Unneutralized sulfonated and / or sulfated compounds are neutralized and mixed with sodium carbonate and water, cooled to 40 ° C. or lower, and then pulverized together with powdery zeolite. Granulate. <Disadvantage> There is a problem of deterioration of an unneutralized product (acid), and excessive water is generated in the neutralization step. When pulverizing and granulating the mixture, an extra step such as lowering to 40 ° C. or lower is required.

4) Japanese Unexamined Patent Publication No. 2-86700: An aqueous surfactant paste and a dry detergency builder are mixed in a surfactant-builder ratio of 0.05: 1 to 1.5: 1 to prepare a dough. After forming, granulation is performed at a granulation temperature of −25 to 20 ° C. <Disadvantage> An extra step of cooling the dough to −25 to 20 ° C. is required for granulation.

5) Japanese Patent Laid-Open No. 61-69900: Spray-dried particles of detergent are crushed and then agitated and granulated in a horizontal mixer in the presence of a surface modifier. <Disadvantage> A step of spray-drying a large amount of surfactant is required, and the organic raw material added in the granulation step is limited to powder and granules other than the binder.

[0009]

As described above, in the conventional method, if the concentration of the surfactant in the mixture is high, good granulation and pulverization cannot be generally performed, so that a cooling step and an aging step are required. Further, when the spray drying method is used, if a surfactant is blended in a high concentration in the system, not only 30 to 40% of water as water must be removed from the slurry, but also the obtained granular detergent It has a low bulk density.

Furthermore, when an acid as a precursor of a surfactant is used as a raw material and this is neutralized before use, it is necessary to take immediate measures such as immediate use and storage at low temperature because of the problem of deterioration. The present invention uses a surfactant salt, which does not easily deteriorate, as a starting material, and mixes most or all of the surfactant into a detergent by a non-spray drying method, without requiring extra steps such as cooling and aging. The present invention provides a method for producing a high bulk density granular detergent which is excellent in free flowing property and contains a surfactant in a high concentration.

[0011]

The method for producing a high bulk density granular detergent according to the present invention comprises the following (a) to (c), wherein the total amount of the granular material obtained by mixing and kneading is 100% by weight. It is characterized in that the components are mixed, kneaded, and then pulverized. (A) Surfactant concentrated paste containing at least one anionic surfactant and having a surfactant concentration of 60% by weight or more: 20 to 55% by weight. (B) Alkali builder containing at least carbonic acid or hydrogen carbonate and potassium salt: 20 to 45% by weight. (C) Spray-dried particles containing zeolite: 5 to the mixture
Amount to add 40% by weight of zeolite.

[0012]

BEST MODE FOR CARRYING OUT THE INVENTION In the present invention, (a) a surfactant-rich paste is used as a main surfactant raw material component. (A) Surfactant concentrated paste contains at least an anionic surfactant, and may contain a nonionic surfactant and the like as necessary. By containing a nonionic surfactant, the viscosity of the paste is reduced, and the paste is made higher in concentration and easier to handle.

As the anionic surfactant, for example, the following ones can be used, and sulfate ester type and sulfonate type are preferable. (1) A linear or branched alkylbenzene sulfonate having an alkyl group or an alkenyl group having an average carbon number of 10 to 18. (2) A higher alcohol sulfate ester salt having an alkyl group or an alkenyl group having an average carbon number of 10 to 18. (3) A higher alcohol ethoxylate sulfuric acid ester salt in which a saturated or unsaturated alcohol residue has an average carbon number of 10 to 18 and an average of 0.5 to 8 mol of ethylene oxide is added in one molecule. (4) An α-olefin sulfonate having an average carbon number of 10 to 18. (5) An α-sulfofatty acid alkyl ester salt in which a saturated or unsaturated fatty acid residue has an average carbon number of 10 to 18 and an alkyl group of the ester has 1 to 5 carbon atoms.

Typical salts are sodium salts and potassium salts. (A) Surfactant concentrated paste contains a total amount of surfactant of 60% by weight or more, preferably 60 to 95% by weight. If this amount is less than 60% by weight, the effect of adding an alkali builder containing carbonic acid or hydrogencarbonate and potassium salts in the powdering step is weakened, and the adhesion of the powdered product and the granular detergent is increased, making handling difficult. Becomes

Examples of the nonionic surfactant include the following. (1) Fatty acid polyoxyethylene alkyl ether represented by the following chemical formula 1

[0016]

[Chemical 1] (R₁CO: saturated or unsaturated fat having 8 to 18 carbon atoms
Acid residue n: shows the average number of moles of oxyethylene added, 8 to 30 R₂: Lower alkyl group having 1 to 5 carbon atoms)

(2) Carbon chain length of saturated or unsaturated alcohol 8 to 18 and average number of added moles of oxyethylene 8
Alcohol ethoxylates of ˜30 (b) As the alkali builder, carbonic acid or hydrogen carbonate and potassium salt, or a mixture of these with other alkali builder is used. The addition ratio of (b-1) carbonic acid or hydrogen carbonate / potassium salt and (b-2) another alkali builder is (b-1) / (b-2) = 99 / by weight.
1 to 20/80 is preferable, more preferably 60/40
~ 35/75.

If the proportion of potassium carbonate in the alkali builder added to the surfactant-rich paste is too low, the resulting powdered product and granular detergent will have increased adhesiveness within the temperature range of the compounding conditions, making handling difficult. Becomes

Examples of the salt of carbonic acid or hydrogen carbonate and potassium include potassium carbonate, potassium sodium carbonate, potassium hydrogen carbonate and the like. As the alkali builder other than carbonic acid or hydrogen carbonate and potassium salt, hydroxides such as sodium carbonate, sodium sesquicarbonate, hydrogen carbonate, potassium hydroxide and sodium hydroxide are preferable.

(C) The spray-dried particles contain zeolite, and may further contain other detergent components. Other detergent components may include a fluorescent agent and its aqueous solution, a pigment and its aqueous solution, sodium sulfite, sodium sulfate, an anionic surfactant, and a nonionic surfactant as a solubility improver. it can. In the present invention, the components are mixed and kneaded at the addition ratios shown in Table 1 below to obtain a kneaded product. However, the addition amount is a value when the total amount of the mixture is 100% by weight.

[0021]

[Table 1] Additive amount Additive amount (a) Surfactant concentrated paste 20-55% by weight 28-52% by weight (b) Alkali builder 20-45% by weight 25-40% by weight (c) Spray-dried particles In the mixture To Zeolite 5 to 45 wt% Zeolite 8 to 36 wt% Blended amount Blended amount

If the amount of the alkali builder with respect to the surfactant paste is too large, the amount of cleaning components in the finally obtained high bulk density granular detergent will decrease and the cleaning power will decrease. Also,
If the amount of the alkali builder is too low, the adhesion of the detergent increases and handling becomes difficult. Also, the amount of zeolite brought into the mixture by the spray-dried particles is 100% detergent composition.
If the amount is less than 5% by weight with respect to the weight%, the adhesion of detergent particles obtained by granulation increases and handling becomes difficult.

Detergent components other than zeolite incorporated in the mixture by spray-dried particles are preferably 13% by weight or less. When a nonionic surfactant is added, it is preferably added in an amount of 0.5 to 15% by weight, more preferably 5 to 12% by weight, in the detergent composition.

The mixing / kneading device used in the practice of the present invention is not particularly limited, but a strong shearing device such as a kneader is preferable. Examples of continuous devices include KRC Kneader (Kurimoto Industry Co., Ltd.) and Honda Continuous Kneader, and examples of batch type devices include vertical kneaders.

By crushing the kneaded product, an average particle size of 3
About 0.00 to 600 μm, bulk density of 0.7 g / cc or more (J
A high bulk density granular detergent according to IS K3362 (6.2)) is obtained. In this crushing step, it is preferable to use a crushing aid such as an aluminosilicate, calcium carbonate or sodium carbonate having an average diameter of 10 μm or less.

Immediately after the production of the high bulk density granular detergent, it is possible to add an inorganic compound such as finely powdered zeocate having a particle size of 10 μm or less as a fluidity improver.
Furthermore, it is also possible to powder blend the detergent particles of the high bulk density granular detergent particles of the present invention with a washing performance improving agent such as a chelate builder and an enzyme. As the chelate builder used here, powdered zeolite, sodium maleate-
Examples thereof include copolymers of acrylic acid and β-alanine sodium diacetate.

[0027]

According to the present invention, (a) a surfactant-rich paste, (b) an alkali builder containing carbonate or a salt of hydrogen carbonate and potassium, and (c) spray-dried particles containing zeolite are mixed and kneaded. The pulverization makes it possible to economically mass produce a high-bulk density granular detergent in a high yield, which is suitable as an industrial production method.

[0028]

【Example】

Example 1 Surfactant paste (surfactant concentration 80.5%) 35.4% by weight (composition: α-sulfofatty acid (C = 14 to 16) methyl ester sodium salt: 22.3% by weight fatty acid (C = 18) polyoxyethylene methyl Ether (EOp = 15): 6.2% by weight Potassium carbonate 11.5% by weight Sodium carbonate 15.0% by weight Spray dried particles 38.1% by weight (Composition: Zeolite: 27.9% by weight α-sulfo fatty acid (C = 14-16) Methyl ester sodium salt : 6.8 wt% Sodium sulfite: 2.8 wt% Fluorescent agent: 0.6 wt%) Total 100.0 wt%

According to the above composition, a spray-dried product containing a surfactant paste, an alkali builder containing potassium carbonate and zeolite was continuously kneaded (Kurimoto Industry Co., Ltd.).
Was kneaded and mixed at 60 ° C., and then molded by a pelletizer. Grinding was carried out after adding 7.0% by weight of finely powdered sodium carbonate having a particle diameter of 10 μm, which is a grinding aid. Further, a fine powder zeolite having a particle size of 10 μm or less was mixed as a fluidity improver to obtain a product. The resulting high bulk density granular detergent has an average particle size of 470 μm and a bulk density of 0.8.
It was 1 g / cc. The results are shown in Table 2. In the above composition, C represents the number of carbon atoms, and EOp represents the average number of added moles of oxyethylene.

Example 2 Surfactant paste (surfactant concentration 75.8%) 28.3% by weight (composition: α-sulfofatty acid (C = 14-16) methyl ester sodium salt: 21.4% by weight) potassium carbonate 14.3% by weight carbonic acid Sodium 18.6 wt% Spray-dried particles 38.8 wt% (Composition: Zeolite: 35.4 wt% Sodium sulfite: 2.9 wt% Fluorescent agent: 0.5 wt%) Total 100.0 wt%

According to the above composition, a spray-dried product containing a surfactant paste, an alkali builder containing potassium carbonate and zeolite was continuously kneaded (Kurimoto Industry Co., Ltd.).
Was kneaded and mixed at 60 ° C., and then molded by a pelletizer. Grinding was carried out after adding 7.0% by weight of finely powdered sodium carbonate having a particle diameter of 10 μm, which is a grinding aid. Further, a fine powder zeolite having a particle size of 10 μm or less was mixed as a fluidity improver to obtain a product. The obtained high bulk density granular detergent has an average particle size of 450 μm and a bulk density of 0.8.
It was 3 g / cc. The results are shown in Table 2.

Example 3 Surfactant paste (surfactant concentration 75.8%) 51.9% by weight (composition: α-sulfofatty acid (C = 14-16) methyl ester sodium salt: 39.3% by weight) potassium carbonate 34.4% by weight carbonic acid Sodium 2.3 wt% Spray-dried particles 11.4 wt% (Composition: Zeolite: 6.4 wt% α-sulfofatty acid (C = 14-16) Methyl ester sodium salt: 1.7 wt% Sodium sulfite: 2.7 wt% Fluorescent agent: 0.6 wt%) Total 100.0% by weight

According to the above composition, a spray-dried product containing a surfactant paste, an alkali builder containing potassium carbonate and zeolite was continuously kneaded (Kurimoto Industry Co., Ltd.).
Was kneaded and mixed at 60 ° C., and then molded by a pelletizer. Grinding was carried out after adding 7.0% by weight of finely powdered sodium carbonate having a particle diameter of 10 μm, which is a grinding aid. Further, a fine powder zeolite having a particle size of 10 μm or less was mixed as a fluidity improver to obtain a product. The obtained high bulk density granular detergent has an average particle size of 490 μm and a bulk density of 0.7.
It was 9 g / cc. The results are shown in Table 2.

Comparative Example 1 Surfactant slurry (surfactant concentration 75.8%) 77.9% by weight (composition: α-sulfofatty acid (C = 14 to 16) methyl ester sodium salt: 59.0% by weight) Sodium carbonate 16.2% by weight Spraying Dry particles 5.9% by weight (Composition: Zeolite: 2.7% by weight α-sulfofatty acid (C = 14-16) Methyl ester sodium salt: 1.1% by weight Sodium sulfite: 1.6% by weight Fluorescent agent: 0.5% by weight) Total 100.0% by weight

According to the above composition, a spray-dried product containing a surfactant paste and sodium carbonate and zeolite as an alkali builder was continuously kneaded (Kurimoto Industry Co., Ltd.).
Was kneaded and mixed at 60 ° C., and then molded by a pelletizer. 7.0% by weight of a finely powdered sodium carbonate having a particle diameter of 10 μm, which is a grinding aid, was added to carry out grinding. The obtained kneaded product had high adhesiveness and the crusher was overloaded, so that high bulk density detergent particles could not be obtained.
The results are shown in Table 2.

[0036]

[Table 2] Example ratio Comparative example 1 2 3 1 Detergent composition (wt%): α-SF * ¹ 22.3 21.4 39.3 59.0 Nonion * ² 6.2 − − − Carbonate K 11.5 14.3 34.4 − Na carbonate 15.0 18.6 2.3 16.2 Zeolite 27.9 35.4 6.4 2.7 Other components (including water) 17.1 10.3 17.6 22.1 Properties: Average particle size 470 450 490 − * ³ Bulk density (g / cc) 0.81 0.83 0.79 − * ³ Manufacturability Good Good Good Overload repose angle 45 40 45- * ³ * 1) α-SF: α-sulfo fatty acid methyl ester sodium salt * 2) Nonion: fatty acid polyoxyethylene alkyl ether * 3) Not measurable

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Yoshihiro Watanabe 1-3-7 Main Office, Sumida-ku, Tokyo Lion Corporation

Claims (1)

[Claims] 1. A total amount of granules obtained by mixing and kneading is 100% by weight, and (a) at least one anionic surfactant is contained, and the surfactant concentration is 60% by weight or more. Surfactant concentrated paste: 20-55% by weight (b) Alkali builder containing at least carbonate or a salt of hydrogen carbonate and potassium: 20-45% by weight (c) Spray-dried particles containing zeolite: 5 to the resulting granules A method for producing a high bulk density granular detergent, which comprises mixing 40% by weight of zeolite in an amount to be blended, kneading and then pulverizing.