JP2000160197A - Production of high bulk density granular detergent - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a sphered high bulk density granular detergent by subjecting detergent granules to a grinding treatment in a specific condition, a treatment using a sieve or an air transportation treatment. SOLUTION: This method for producing the bulk density granular detergent comprises applying at least one sphering treatment method selected from the following treatments (a), (b) and (c) to detergent granules to sphere the detergent granules: (a) the detergent granules are sphered with a grinding machine having a grinding rotator having a circumferential rate of 25-50 m/s; (b) the detergent granules are sphered with a sieve at a shaking rate of 60-3,000 shakes/min; and (c) the detergent granules are sphered by the transportation of air in a condition under a condition of a fluid number of 8-30.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

FIELD OF THE INVENTION The present invention relates to a method for producing a sphered high bulk density granular detergent.

[0002]

2. Description of the Related Art In recent years, in the field of detergents for clothes, surfactants, which are generally referred to as compact detergents and have a high concentration of surfactants, and have a large bulk density, have become the mainstream. High bulk density granular detergents are manufactured by kneading, crushing granulation, stirring granulation, etc., but the resulting detergent particles are generally indefinite and not necessarily spherical in shape. Was.

[0003]

In high bulk density granular detergents, if the irregularity of the detergent particles becomes remarkable, the appearance, the bulk density, the flowability (the angle of repose becomes large), etc., of the product will decrease. Cause problems. Then, an object of the present invention is to solve such a problem and to produce a spherical high bulk density granular detergent composition. In addition, there are the following related arts related to the present invention, but none of them suggest the present invention.

(1) JP-A-63-150392:
Using a cutter mill type pulverizer having a screen classification function, the kneaded product of the detergent component is sequentially supplied from a pulverizer having a large screen hole diameter to a small pulverizer to perform multi-stage pulverization to produce a high bulk density granular detergent. However, this conventional document does not describe the point of performing the sphering process, and does not suggest the present invention. Further, the peripheral speed of the cutter of the crusher of the embodiment is 24 m / s, which is different from the present invention.

(2) JP-A-7-268398: In producing nonionic surfactant particles by stirring granulation, zeolite or silica is dividedly charged to control granulation physical properties. The granulation was performed by a Lodige mixer, the peripheral speed of the stirring blade was 55 m / s, irregular particles were obtained, and the spheroidizing treatment as in the present invention was not suggested.

(3) JP-A-8-283788: α
-Addition of an anti-adhesion agent such as zeolite to a granulated product containing a sulfo fatty acid alkyl ester alkali metal salt and pneumatically transport the granulated product to produce a high bulk density granular detergent. However, the technique described in this known document aims at pneumatic transportation while preventing detergent granules from adhering to transportation pipes, and pneumatic transportation processing under specific conditions for the purpose of spheroidization processing. It does not suggest the present invention utilizing The Froude number in the example of this known document is 43, which is different from the present invention.

(4) JP-A-8-337323: When transporting bleach particles by pneumatic transportation, the bleach particles are transported in a region of a fluid number of 3 to 11 to prevent the generation of fine powder. The processing object and processing purpose are different from those of the present invention. (5) JP-A-2-255800: bleach activator,
A bleach activator composition comprising a nonionic surfactant and a carbonate in a specific ratio is described. Only treatment with a marmellaiser is described and does not suggest the present invention.

[0008]

Means for Solving the Problems The method for producing a high bulk density granular detergent of the present invention comprises the following steps (a),
The method is characterized in that at least one sphering means of (b) or (c) is applied to produce a high bulk density granular detergent comprising spheroidized detergent particles. (A) The detergent granules are subjected to spheroidizing treatment with a crusher having a crushing rotating body having a peripheral speed of 25 to 50 m / s. (B) The detergent granules are subjected to spheroidizing treatment with a sieve vibrating at 60 to 3000 times / minute. (C) A spheroidizing treatment is performed by pneumatic transportation under the conditions of a Froude number of 8 to 30.

[0009]

BEST MODE FOR CARRYING OUT THE INVENTION According to the present invention, detergent granules are subjected to spheroidizing treatment by at least one of the following treatments. (A) The spheroidizing treatment is performed with a crusher under specific conditions. (B) spheroidizing with a sieve under specific conditions. (C) A spheroidizing treatment is performed by pneumatic transportation under specific conditions. The subject of this spheroidizing treatment is a detergent granule, and the detergent granule is a conventional method, for example, a stirring type mixing device capable of mixing a surfactant such as a nonionic surfactant and a detergent builder,
Preferably, a stirring type mixing device capable of mixing a surfactant such as a nonionic surfactant and a detergent builder while consolidating the same is used. For example, it is manufactured by the following method.

(1) By kneading (kneading) a detergent raw material or by extruding and cutting,
Alternatively, it can be obtained by crushing the kneaded product (kneaded product) or extruded product with a crusher. As a specific device, a kneader such as a kneader, an extruder having a pelletizer, a cutter, or the like, a coarse pulverizer, or the like is used to obtain a detergent granule (for example, 300 μm or more). (2) A detergent granule (for example, 300 μm or more) is obtained by a stirring granulator such as a Ladyge mixer. (3) Detergent granules (for example, 300 μm or more) are obtained by a rolling granulator such as a horizontal rotating drum.

The detergent granules of the present invention can use conventional detergent raw materials, and may optionally contain surfactants such as nonionic surfactants and anionic surfactants, cleaning builders, and other additional components. Yes, the composition is not particularly limited. Preferably, the nonionic surfactant is suitably used for producing a granular detergent containing 10 to 50% by weight of a nonionic surfactant and having a nonionic surfactant as a main active ingredient.
It can also be used for the production of granular detergents containing up to 50% by weight and having an anionic surfactant as the main activator component.

Preferred nonionic surfactants include, for example, the following. An alkylene oxide having 2 to 4 carbon atoms is added to an aliphatic alcohol having 6 to 22 carbon atoms, preferably 8 to 18 carbon atoms, preferably 3 to 3 carbon atoms on average.
0 mol, preferably 5 to 20 mol, of a polyoxyalkylene alkyl (or alkenyl) ether added. Among them, polyoxyethylene alkyl (or alkenyl) ether and polyoxyethylene polyoxypropylene alkyl (or alkenyl) ether are preferable. As the aliphatic alcohol used here, the first
A secondary alcohol or a secondary alcohol is used. Further, the alkyl group may have a branched chain. As preferred aliphatic alcohols, primary alcohols are used.

Polyoxyethylene alkyl (or alkenyl) phenyl ether. For example, a fatty acid alkyl ester alkoxylate represented by the following general formula (I) in which an alkylene oxide is added between ester bonds of a long-chain fatty acid alkyl ester.

Embedded image R ¹ CO (OA) nOR ² ... (I) (R ¹ CO: a fatty acid residue having 6 to 22 carbon atoms, preferably 8 to 18 carbon atoms OA: 2 to 4 carbon atoms such as ethylene oxide and propylene oxide; Preferably 2 to 3 additional units of alkylene oxide n: average number of moles of alkylene oxide added, generally 3 to 30, preferably 5 to 20 R ² : having a substituent having 1 to 3 carbon atoms Lower alkyl group)

Polyoxyethylene sorbitan fatty acid ester. Polyoxyethylene sorbite fatty acid ester. Polyoxyethylene fatty acid esters. Polyoxyethylene hydrogenated castor oil. Glycerin fatty acid esters. Fatty acid alkanolamides.

Among the above nonionic surfactants, polyoxyethylene alkyl (or alkenyl) ether, polyoxyethylene polyoxypropylene alkyl (or alkenyl) ether having a melting point of 40 ° C. or less and an HLB of 9 to 16, fatty acid methyl ester Fatty acid methyl ester ethoxylate in which ethylene oxide is added to fatty acid, and fatty acid methyl ester ethoxypropoxylate in which ethylene oxide and propylene oxide are added to fatty acid methyl ester are preferably used. Further, these nonionic surfactants may be used as a mixture.

Examples of the anionic surfactant include a linear or branched alkyl (average carbon chain length of 8 to 18) benzene sulfonate and a long-chain alkyl (average carbon chain length of 10 to 2).
0) Sulfonate, long chain olefin (average carbon chain length 10
-20) sulfonate, long-chain monoalkyl (average carbon chain length 10-20) sulfate ester salt, polyoxyethylene (average degree of polymerization 1-10) long-chain alkyl (average carbon chain length 1)
0-20) ether sulfates, polyoxyethylene (average degree of polymerization 3-30) alkyl (average carbon chain length 6-
12) Phenyl ether sulfate, α-sulfo fatty acid alkyl ester (average carbon chain length of fatty acid residue 1
2-20), long-chain monoalkyl, dialkyl or sesquialkyl phosphate, polyoxyethylene monoalkyl, dialkyl or sesquialkyl phosphate, soap and the like. These anionic surfactants can be used as alkali metal salts such as sodium and potassium, amine salts, ammonium salts and the like. Further, the above-mentioned surfactants can be used as one kind or as a mixture of two or more kinds.

Other detergent components include cationic surfactants, amphoteric surfactants, zeolites, chelate builders such as sodium tripolyphosphate and sodium pyrophosphate; sodium citrate, sodium ethylenediaminetetraacetate, nitrilotriacetate, Organic builders such as sodium acrylate, sodium acrylate-sodium maleate anhydride copolymer, polyacetal carboxylate, sodium hydroxyiminodisuccinate; sodium carbonate, potassium carbonate, sodium hydrogen carbonate, potassium hydrogen carbonate, sodium silicate, crystalline Alkaline builders such as silicates; anti-redeposition agents such as carboxymethyl cellulose and polyethylene glycol; para-toluenesulfonate, toluenesulfonate, xylenesulfonate, urea, etc. Degrees modifier; quaternary ammonium salts,
Softener additives such as bentonatoy; neutral inorganic salts such as sodium sulfate; reducing agents such as sodium sulfite and sodium bisulfite; bleaching agents such as sodium percarbonate and sodium perborate; ethylenediaminetetraacetate; octanoyloxybenzenesulfonic acid Bleaching activators such as sodium, optical brighteners, flavors, proteases, lipases,
Examples include enzymes such as cellulase, dyes, white carbon, and the like.

In a granular detergent composition containing a nonionic surfactant as a main active component, it is preferable to add a clay mineral, an oil-absorbing carrier, and the like.
No. 87691 describes this in detail. Specifically, as a clay mineral, for example, a clay mineral having a dioctahedral type three-layer structure includes montmorillonite, nontronite, beidellite, pyrophyllite, and the like, while a trioctahedral type three-layer structure is taken. Examples of clay minerals include saponite, hectorite, stevensite, and talc. Particularly preferred clay minerals include Na-type montmorillonite, Ca-type montmorillonite, activated bentonite (N
a / Ca-type montmorillonite), Na-type hectorite,
Ca-type hectorite. The clay mineral is contained in the granular nonionic detergent composition preferably at 0.1 to 30% by weight, more preferably 1 to 20% by weight, and particularly preferably 3 to 10% by weight.

The oil-absorbing carrier is added to suppress the exudation of nonions and solidification of the detergent particles under high temperature and high humidity, and to improve the solubility of the detergent when the detergent is used. The oil-absorbing carrier is a porous fine powder sufficient to adsorb and retain the nonionic surfactant, and physically adsorbs the nonionic surfactant, but does not swell due to it. The oil absorption of the oil absorbing carrier used in the present invention is larger than that of the clay mineral. Examples of such an oil-absorbing carrier include, for example, amorphous silicic acid (Toxor made by Toxor,
Aerosil made by Nippon Aerosil, Nip Seal made by Nippon Silica, amorphous calcium silicate (Aloxite made by Toxor, Thixorex made by Kofran Chemical), amorphous aluminosilicate, magnesium silicate, magnesium carbonate, calcium carbonate, spinel, cordierite , Mullite, starch decomposition products (Pine Flow, manufactured by Matsutani Chemical), and the like. These oil-absorbing carriers may be used as a mixture. The oil-absorbing carrier is suitably blended in a high bulk density granular nonionic detergent in an amount of 0.1 to 20% by weight, preferably 0.5 to 15% by weight, and more preferably 1 to 15% by weight.
10% by weight is blended.

Next, the sphering process will be described. (A) Spherification treatment with a crusher at a specific peripheral speed (25 to 50 m / s) Suitable for producing a granular detergent containing a nonionic surfactant as a main active ingredient. In producing a high bulk density granular detergent containing a nonionic surfactant as a main component, if crushed under specific conditions using a crushing granulator, nonionic detergent particles can be made spherical without impairing solubility, As a result, the flow characteristics are improved. The phenomenon that can be spheroidized by the crushing granulator is considered to be a peculiar phenomenon due to the viscosity and elasticity of the nonionic detergent particles. As the sphering apparatus, generally, a crushing granulator equipped with a rotating body and a screen inside, preferably, a hammer mill, an atomizer, an impact crusher such as a pulperizer,
A cutting / shearing crusher such as a cutter mill or a feather mill is used, and examples thereof include a Fitz mill (manufactured by Hosokawa Micron Corporation) and a speed mill (manufactured by Okada Seiko Co., Ltd.).

The crusher may be of any type, but as shown in FIG.
One that discharges spherical detergent granules pulverized by the rotary crushing blade 19 and formed into a spherical shape from the screen 17 having a predetermined hole diameter is preferably used. The detergent granules are supplied from the supply port 13 to the crushing chamber 11 via the rotary valve 14, and the crushed and spherical detergent particles are discharged from the discharge port 21 through the hole diameter (opening) of the screen 17. You. During the crushing process, cooling air is supplied from the cooling air supply port 15 to the crushing chamber 1.
1 is supplied. In the crushing treatment, it is preferable to add a fine powder having an average particle size of 50 μm or less as a crushing aid or a coating agent. As this fine powder, aluminosilicate such as zeolite, sodium carbonate,
Carbonates such as carnium carbonate, amorphous silica, silicates such as calcium silicate and magnesium silicate, and the like can be used.

The peripheral speed of the rotating body of the crushing granulator is 25 to 5
0 m / sec, preferably 30 to 48 m / sec
c, more preferably 32 to 46 m / sec. When the peripheral speed is 25 m / sec or less, the spheroidization is deteriorated, and the particle size distribution of the obtained detergent particles becomes broad. On the other hand, even if it exceeds 50 m / sec, the spheroidization of the obtained detergent particles deteriorates.

(B) Specific vibration (60 to 3000 times /
Spheroidizing treatment with sieve of (ii) The sieve used is preferably a flat sieve or a vibrating sieve. The plane sieve is a sieve that gives a reciprocating motion to a slightly inclined plane sieve almost parallel to the surface. A vibrating sieve is a sieve that gives a rapid vibration in a direction substantially perpendicular to the sieve surface. In any case, it is preferable to use a sieve having a mesh size of 2 to 4 times the average particle size of the particles to be subjected to the sieve. Further, it is desirable that the time for the sieve is at least 5 seconds. Specific examples of such a sieve include Lotex Screener (Seishin K.K.) and Dalton Vibrating Sieve (Dalton Co., Ltd.). Vibration by a sieve is 60 to 3000 times / minute, preferably 10 to 3000 times / minute.
0 to 2500 times / minute, more preferably 150 to 2000
Given by vibrations per minute. If the frequency of the sieve is less than 60 times / minute, the sieve cannot be formed into a sphere and the solubility and fluidity deteriorate. On the other hand, if it exceeds 3000 times / minute, spheroidization cannot be performed, and dust generation in the device also increases.

The method using a sieve of the present invention is particularly effective for spheroidizing a high bulk density granular detergent containing a nonionic surfactant as a main active ingredient. By sieving at a temperature higher than the melting point of the nonionic surfactant, spheroidization is further promoted, which is desirable. In the sieving step, coarse powder larger than the desired material remaining on the sieve is crushed and mixed with the intermediate powder. Fine powder smaller than the desired material that has passed through the sieve can be returned to the granulator again and used as a raw material for granulation.

(C) Specific conditions (Froude number 8 to 30)
FIG. 2 is a schematic view showing an example of the pneumatic transport process of the present invention, in which the detergent granulated product is pneumatically transported by a transport pipe. The spheronized granules after the spheronization treatment (the high bulk density granular detergent of the present invention) are collected by the cyclone. Exhaust gas and accompanying detergent fines are exhausted by an exhaust blower. The detergent fines are collected by a dust collector, supplied as a part of the raw material in the detergent granulation step, and can be reused. In the present invention, the detergent granule is used for a fluid number of 8 to 3
Pneumatic transportation is performed under the condition of 0, preferably 10 to 30. If the Froude number is less than 8, spheroidization is not sufficient, and the detergent particles cannot be transported efficiently. On the other hand, when the Froude number exceeds 30, the detergent particles are broken by impact.

The Froude number is defined by the following equation (I).

(Equation 1) u: transport wind speed (m / sec.) D: inner diameter of transport pipe (m) gc: gravitational acceleration (9.8 m / sec. ² )

The ratio of the transport air (air) to the detergent granules (solid) and the air / solid ratio are preferably 0.5 to 5 by volume, more preferably 0.5 to 4. If this ratio is too small, the transport piping tends to be blocked. On the other hand, if it is too large, the friction between the detergent particles decreases, and the spheroidizing effect decreases. The average residence time of the detergent granules in the transport pipe is at least 1 second, preferably 1.5 to 10 seconds. When the detergent granules containing a nonionic surfactant as a main active ingredient are made spherical by pneumatic transportation, the temperature of the transportation air can be selected in a wide range, and for example, transportation air of 10 to 60 ° C. is used. When the detergent granules containing an anionic surfactant as the main active ingredient are transported by air, the temperature of the transport air is 30 to 5
0 ° C. is preferred. If this temperature is too low, the plasticity of the surfactant is not sufficiently exhibited, and the spheroidizing effect is small. On the other hand, 50
If the temperature exceeds ℃, the detergent particles tend to adhere to the transportation pipe.

Although the principle of spheroidization during pneumatic transportation is not clear, it is presumed to be due to the plasticity of the activator acting as a binder. When the anionic surfactant is the main base, it is considered that plasticity is exhibited by setting the air temperature to the above-mentioned temperature. Collision, friction between detergent particles,
Alternatively, it is considered that spheroidization progresses due to collision and friction with the transport piping wall.

The average particle size of the high bulk density granular detergent of the present invention is as follows:
300 to 3000 μm is suitable, preferably 400 to
２０００2000 μm. The bulk density of the high bulk density granular detergent of the present invention is suitably from 0.6 to 1.3 g / ml, preferably from 0.7 to 1.2 g / ml. Further, in the present invention, the above-mentioned sphering means can be applied in combination, and a preferred method is a method of sequentially performing processing as described below. Among these, the methods (C) and (D) are preferable. (A): (a) Spherification treatment by crusher → (c) Spherification treatment by pneumatic transportation is sequentially performed. (B): (c) Spherification treatment by pneumatic transportation → (a) Spherification treatment by a crusher is sequentially performed. (C): (a) sphering treatment by a crusher → (c) sphering treatment by pneumatic transportation → (b) sphering treatment by a sieve. (D): (c) sphering treatment by pneumatic transportation → (a) sphering treatment by a crusher → (b) sphering treatment by a sieve.

[0030]

According to the present invention, a sphered high bulk density granular detergent can be obtained by crushing, sieving or pneumatically transporting the detergent granules under specific conditions.

[0031]

EXAMPLES Examples 1 to 6: Spherification treatment by a crusher [Production method A] Nonionic surfactant, washing builder, bentonite and white carbon were supplied to a Ledige mixer (M-20, manufactured by Matsubo Corporation). 1 mm
The above detergent mass was prepared. Then, a hammer mill (TAHM-M manufactured by Tokyo Atomizer Co., Ltd.) equipped with a screen having a hole diameter of 2.5 mmφ was used for the detergent mass and the fine powder.
8 hammer diameter 0.45 m), crushed and granulated to give a spheroidizing treatment. Finally, the surface of the granulated product was coated with a fine powder to obtain a high bulk density granular nonionic detergent.

[Production Method B] A nonionic surfactant, a washing builder, bentonite, and white carbon were charged into a continuous kneader (S-4, Kurimoto Iron Works Co., Ltd.), and 1
A detergent mass of not less than mm was prepared. Next, the detergent lump and the fine powder were subjected to a cutter mill equipped with a screen having a hole diameter of 2 mmφ (Fitzmill D manufactured by Hosokawa Micron Corporation).
KA6 type, cutter diameter 0.2634m)
Crushing and granulation were performed and spheronization treatment was performed. Finally, the surface of the granulated product was coated with a fine powder to obtain a high bulk density granular nonionic detergent.

[Production method C] A continuous kneader (Kurimoto Iron Works Co., Ltd. model S-4) together with a washing builder, bentonite and white carbon as in production method B, using an anionic surfactant instead of a nonionic surfactant. 1mm
The above detergent mass was prepared. Next, the detergent lump and the fine powder were subjected to a cutter mill equipped with a screen having a hole diameter of 2 mmφ (Fitzmill DKA manufactured by Hosokawa Micron Corporation).
6 and a cutter diameter of 0.2634 m), and crushed and granulated to give a spheroidizing treatment. Finally, the surface of the granulated product was coated with a fine powder to obtain a high bulk density granular nonionic detergent.

Using the compositions shown in Table 1 below, high bulk density granular detergents were produced according to the above Production Methods A, B and C, respectively, and the sphericity was evaluated according to the following criteria. In addition, the angle of repose, the bulk density, the average particle size, and the particle size distribution were measured, and these are shown in Table 1. The details of the raw materials used in Table 1 are as follows.

[Sphericity test] A photomicrograph of about 100 detergent particles was arbitrarily taken, and the Heywo of each of the particles was taken.
The minor axis and major axis are measured according to the definition of “od”. The ratio, that is, the ratio of minor axis / major axis ≧ 0.95 was calculated. ◎: 80% or more ○: 60 to 80% △: 40 to 60% ×: 40% or less

[Raw materials] Nonionic surfactant (1) Nonionic surfactant AC ₁₂ H ₂₅ O (CH ₂ CH ₂ O) ₆ H (2) Nonionic surfactant BC ₁₆ H ₃₃ CO (OCH ₂ CH) ₂ ) ₉ OCH ₃ cleaning builder (1) Cleaning builder A zeolite A type (Silton B manufactured by Mizusawa Chemical Co., Ltd.) (2) Cleaning builder B sodium carbonate (manufactured by Asahi Glass Co., Ltd.) Fine powder (1) Fine powder AP Zeolite (Crossfield, average particle size 1)
(2) Fine powder B calcium carbonate (Shiraishi Industry Co., Ltd., average particle diameter 3μ)
m) Bentonite: Ca bentonite (LAUNDROSIL manufactured by Nissan Gardler Catalysts Co., Ltd.) White carbon: amorphous silica (Tokusil NR manufactured by Tokuyama Corporation) LAS: potassium dodecylbenzenesulfonate

[0037]

[Table 1] Table 1: Spheronization treatment using a crusher Example Comparative Example 1 2 3 4 5 6 1 2 Composition (% by weight) Nonionic surfactant: A 20 20 20 20 20 -20 20: B 5 5 5 5 5-5 5 Washing builder: A 20 20 20 20 20 20 20 20: B 25 25 25 25 25 25 25 25 25 Fine powder (for crushing and granulation): A 8-8-8 8 8 8: B-8- 8 − − − − Fine powder (for coating): A 2 − 2 − 2 2 2 2: B − 2 − 2 − − − − − Bentonant 8 8 8 8 8 8 8 8 White carbon 4 4 4 4 4 4 4 4 LAS------25-- Other minor components Balance (manufacturing conditions) Manufacturing method AABBBCAB Crusher peripheral speed (m / sec) 27.5 31 39 47 49 39 20 55 (Evaluation result) Sphericity △ ○ ◎ ○ △ ○ × × Angle of repose (°) 40 37 35 38 40 38 45 45 Bulk density (g / ml) 0.88 0.90 0.92 0.90 0.88 0.83 0.85 0.85 Average particle diameter (μm) 500 520 500 510 490 500 500 500 1000 μm or more Particles (%) 10 6 5 5 4 6 16 2 Particles smaller than 150 μm (%) 10 5 4 5 6 6 14 8

Examples 7 to 12: Spherification treatment with a sieve A high bulk density granular detergent composition containing a nonionic surfactant as a main active ingredient was prepared according to the composition shown in Table 2 below, and evaluated by the following method. The results are shown in Table 2. [Manufacturing method] The powdery raw materials shown in Table 2, namely, zeolite, amorphous silica and sodium carbonate were charged into a Lodige mixer (M20, manufactured by Matsuzaka Giken Co., Ltd.), and a main shaft (200 rpm) and a chopper ( (6000 rpm) stirring was started. The amount of the nonionic surfactant shown in Table 2 was added thereto for 1 minute, followed by stirring and granulation. During the stirring, sampling was carried out with time, and when the average particle diameter reached 460 μm, 5% of fine zeolite was added as a fluidity improver to obtain an irregular detergent granule. This amorphous granulated product was evaluated for sphericity in the following spheronization test, and had an average particle size of 460 μm. Then, sieving was performed using the following equipment to obtain spherical particles. The processing conditions are shown in Table 2. Apparatus A: Dalton vibrating sieve, aperture 1410 μm Equipment B: Lotex cleaner, aperture 1190 μm Finally, the enzyme was powder-mixed to give a final high bulk density granular nonionic detergent.

[Raw Materials] Nonionic surfactant: C ₁₂ H ₂₅ (CH ₂ CH ₂ O) ₇ H
(Polyoxyethylene lauryl ether obtained by adding an average of 7 moles of ethylene oxide to Connol 20P manufactured by Nippon Rika Co., Ltd.), melting point: about 12 ° C. White carbon: amorphous silica (Tokushil N manufactured by Tokuyama Corporation) Enzyme: Lipase / Protease / cellulase / alcalase = 1/1/1/1 mixture Fluorescent agent: 4,4'-bis (2-sulfostyryl) biphenyl disodium (Tinopearl CBS-X manufactured by Ciba Specialty Chemicals) [Small amount in other components Some of the additives]

[Sphericity test] A photomicrograph of approximately 100 detergent particles was taken arbitrarily, and each of the particles was subjected to Heywo.
The minor axis and major axis are measured according to the definition of “od”. The ratio, that is, the ratio of minor axis / major axis ≧ 0.95 was calculated. ◎: 80% or more ○: 60 to 80% △: 40 to 60% ×: 40% or less

[Solubility test] 5 in a 1-liter beaker
℃ 24 tap water, JIS24 mesh pass ~ JI
5g of detergent particles of S32 mesh on are charged, and for 5 minutes,
The mixture was stirred under the condition of 25 rpm. Thereafter, the remaining detergent particles are taken out on a nylon cloth,
After drying for one minute, the weight was measured, and the dissolved residue was calculated from the following equation (II) to obtain a solubility index.

## EQU2 ## Dissolved residue (%) = {dissolved residue amount (g) / 5 (g)} × 100 (II) ：: 0% ≦ dissolved residue <1% ○: 1% ≦ dissolved residue <5% Δ: 5% ≦ dissolution residue <10% X: 10% ≦ dissolution residue

[Fluidity test] Based on JIS Z2502, the angle of repose at room temperature was measured by a discharge method. ：: 50 ° or less ○: 50 ° to 60 ° △: 60 ° to 65 ° ×: 65 ° or more

[0043]

[Table 2] Table 2: Spherification treatment by sieve Example Comparative Example 7 8 9 10 11 12 34 4 composition (% by weight) Nonionic surfactant 22 22 22 22 22 22 22 22 A type zeolite 27 27 27 27 27 27 27 27 Sodium carbonate 35 35 35 35 35 35 35 35 White carbon 4 4 4 4 4 4 4 4 Glauber's salt 3 3 3 3 3 3 3 3 Enzyme 1 1 1 1 1 1 1 1 1 Other components Balance manufacturing conditions Equipment A (times / minute) 70 1000 2800-1000 1000 50 3200 Equipment B (times / minute)---300----Temperature (° C) 20 20 20 20 12 12 12 12 Sieve residence time (seconds) 5 30 10 7 60 10 10 10 Evaluation result Bulk density (g / ml) 0.92 0.94 0.92 0.92 0.92 0.90 0.88 0.88 Average particle size (μm) 450 440 450 440 450 460 460 460 sphericity ○ ◎ ○ ◎ ○ △ × × Solubility ○ ◎ ◎ ◎ ◎ ◎ × ◎ Fluidity ○ ◎ ◎ ◎ ◎ ◎ △ ◎

Examples 13 and 14: Spherification treatment by pneumatic transportation (1) Preparation of high bulk density granular nonionic detergent Nonionic surfactant [C ₁₂ H ₂₅ (CH ₂ CH ₂ O) ₇ H
(Polyoxyethylene lauryl ale obtained by adding an average of 7 moles of ethylene oxide to Connol 20P manufactured by Nippon Rika Co., Ltd., melting point: about 12 ° C.) Amorphous silica [white carbon: Toksil N (manufactured by Tokuyama Corporation)] 4 weight Part, 20% by weight of bentonite,
20% by weight of sodium carbonate, 25 parts by weight of A-type zeolite, and a fluorescent agent (Tinopearl CBS manufactured by Ciba-Geigy / Whytex SKC = 5/1 mixture manufactured by Sumitomo Chemical Co., Ltd.) are kneaded using a continuous kneader (KRC2 type, Kurimoto Iron Works). The kneaded product obtained by kneading and kneading, and zeolite 5 as a grinding aid
Weight parts are fimil (Hosokawa Micron DKASO6
) To obtain a detergent granulated product (unshaped product). This irregular shaped detergent granulated product was used as Comparative Example 5. Further, the detergent granules (irregular shaped products) were pneumatically transported using the apparatus shown in FIG. This pneumatic transportation was repeated five times to obtain a nonionic detergent of Example 13 of the present invention. The sphericity and the angle of repose of the detergents of Example 13 and Comparative Example 5 were evaluated, and the results are shown in Table 3. The method of evaluating the sphericity and the angle of repose is the same as in Examples 7 to 12.

Preparation of High Bulk Density Granular Anionic Detergent A slurry containing each component and having a water content of 50% was spray-dried using a countercurrent spray dryer at a hot air temperature of 230 ° C.
The product was dried to a dry water content of 5% to prepare a spray-dried product containing the following components. Sodium salt of α-sulfofatty acid methyl ester (12-14 carbon atoms of fatty acid residue / 16-18 carbon atoms = 3-7
(Weight ratio) mixture): 5 parts by weight Potassium linear alkyl (C ₁₀ -C ₁₄ ) benzenesulfonate: 20 parts by weight Potassium α-olefin sulfonate C ₁₄ -C ₁₈ : 3 parts by weight Soap: 4 parts by weight Carbonic acid Potassium: 6 parts by weight Sodium carbonate: 9.8 parts by weight Sodium sulfite: 2 parts by weight Sodium silicate: 2 parts by weight Zeolite: 18 parts by weight Fluorescent agent: 0.2 parts by weight Water: 5 parts by weight

Next, 3 parts by weight of a nonionic surfactant (25 mol adduct of ethylene oxide of a primary alcohol having 12 to 13 carbon atoms), 2 parts by weight of potassium carbonate, 12 parts by weight of sodium carbonate were added to 75 parts by weight of the spray-dried product. 6 parts by weight of zeolite and 2 parts by weight of added water were added, and the mixture was kneaded with a KRC kneader (Kurimoto Iron Works Co., Ltd.) and formed into pellets of about 10 mmφ × 20 mm with an extruder (manufactured by Fuji Paudal). The pellet product is crushed and granulated by a speed mill (manufactured by Okada Seiko Co., Ltd.) equipped with a screen.
Obtained detergent granules (irregular shaped product)

This irregular shaped detergent granulated product was used as Comparative Example 6. Further, the detergent granules (irregular shaped products) were pneumatically transported using the apparatus shown in FIG. This pneumatic transport was repeated five times to obtain the anionic detergent of Example 14 of the present invention. The sphericity and angle of repose of the detergents of Example 14 and Comparative Example 6 were evaluated, and the results are shown in Table 3.

[0048]

Table 3: Spheronization treatment by pneumatic transport Nonionic detergent Anionic detergent Example 13 Comparative Example 5 Example 14 Comparative Example 6 Average particle size (μm) 500 500 560 560 Bulk density (g / ml) 0.90 0 0.90 0.85 0.85 Air velocity (m / s) 20-20-Froude number 28.5-28.5-Air temperature (° C) 20-37-Sphericity ◎ × ◎ × angle of repose (°) 35 ~ 40 45 45 45-50

Embodiments 15 to 18 A plurality of sphering means are combined to perform sphering processing.
Table 4 shows the results.

Table 4: Sphering means and evaluation results Example 15 Example 16 Example 17 Example 18 Composition of detergent Same sphering means as in Example 3 Crushed air transport Crushed air transport (Example 3) (Same as Example 13 (same as Example 3 (same as Example 13)) ↓ ↓ ↓ ↓ ↓ Pneumatic transport Crushing Pneumatic transport Crushing (Example 13 (Example 3 (Example 13 (Example 13 ↓ ↓ Sieve (same as Example 8 ( same as Example 8 )) Evaluation result Sphericity ◎ ◎ ◎ ◎ Bulk density (g / ml) 0.94 0.93 0.95 0.94 Average particle size (μm) 480 490 470 480 Solubility ◎ ◎ ◎ ◎ Fluidity 33 34 30 33 Particles of 1000 μm or more (%) 4 5 4 4 Particles of less than 150 μm (%) 4 4 4 4

[Brief description of the drawings]

FIG. 1 is an explanatory view showing an embodiment of a crusher used in an embodiment of the present invention.

FIG. 2 is an explanatory diagram showing an embodiment of a pneumatic transportation device used in the embodiment of the present invention.

[Explanation of symbols]

 REFERENCE SIGNS LIST 11 crushing chamber 13 supply port 14 rotary valve 15 cooling air supply port 17 screen 19 rotary crushing blade 21 discharge port

 ──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Tomonori Takahashi 1-3-7 Honjo, Sumida-ku, Tokyo Inside Lion Corporation (72) Inventor Hiroyuki Iwabuchi 1-3-7, Honjo, Sumida-ku, Tokyo F-term in Lion Corporation (reference) 4H003 AB19 AB44 AC08 AC12 BA10 CA20 DA01 EA16 EA25 EA27 EA28 EA30 FA41

Claims (1)

[Claims] 1. The following (a),
A method for producing a high bulk density granular detergent, comprising subjecting at least one sphering treatment means selected from (b) and (c) to spheroidizing a detergent granule. (A) The detergent granules are subjected to spheroidizing treatment with a crusher having a crushing rotating body having a peripheral speed of 25 to 50 m / s. (B) The detergent granules are subjected to spheroidizing treatment with a sieve vibrating at 60 to 3000 times / minute. (C) A spheroidizing treatment is performed by pneumatic transportation under the conditions of a Froude number of 8 to 30.