JPH11293290A - Method for producing granular nonionic detergent composition - Google Patents

Abstract

(57) [Problem] To provide a method for producing a granular nonionic detergent composition capable of maintaining a good odor (odor) even after long-term storage. SOLUTION: In producing a granular nonionic detergent composition containing at least a nonionic surfactant, a cleaning builder, and a fragrance, the nonionic surfactant and the fragrance are mixed in advance, and then the mixture and the cleaning builder are stirred, granulated or kneaded. Wag granulation.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates to a method for producing a granular nonionic detergent composition, and more particularly to a method for producing a granular nonionic detergent composition capable of maintaining a good odor even after long-term storage.

[0002]

2. Description of the Related Art Nonionic surfactants generally have a low foaming property, and their detergency is hardly affected by the hardness of water. Furthermore, it is an excellent surfactant having good biodegradability, low environmental load, low toxicity and no problem in safety. However, nonionic surfactants have a unique unpleasant odor due to trace amounts of lower alcohols and lower fatty acids usually contained,
For this reason, there is a problem that a solid detergent composition containing a nonionic surfactant generates an unpleasant odor at the time of dissolution or the like, thereby deteriorating the feeling of use of the product.

Therefore, it is conceivable to mask the unpleasant odor of the nonionic surfactant by blending the fragrance into the detergent composition. However, the blending amount of the nonionic surfactant in the detergent composition is much larger than the blending amount of the fragrance. In order to completely mask the unpleasant odor of the nonionic surfactant, a large amount of a fragrant fragrance must be added, and as a result, the fragrance of the detergent composition becomes too strong or the detergent composition There has been a problem that it becomes difficult to continue masking the strong unpleasant odor generated during dissolution. Therefore, a composition has been proposed in which a specific fragrance component is blended to mask the unpleasant odor of the nonionic surfactant without excessively intensifying the scent of the composition (JP-A-5-202387). .

[0004] In addition, the nonionic detergent composition containing a fragrance has a problem that the fragrance (aroma) is deteriorated during storage. In particular, since the compounding amount is controlled so that the fragrance of the composition does not become too strong, deterioration of the fragrance becomes a serious problem.

[0005]

SUMMARY OF THE INVENTION Accordingly, the present invention has been made in view of the above-mentioned circumstances of the prior art, and has a granular nonionic detergent composition capable of maintaining a good odor even after long-term storage. An object of the present invention is to provide a method for manufacturing a product.

[0006]

Means for Solving the Problems As a result of intensive studies, the present inventors have prepared a nonionic-perfume mixture by previously mixing a nonionic surfactant and a perfume, and then mixing the nonionic surfactant with a washing builder. The present inventors have found that the above objects can be achieved by subjecting the particles to a grain treatment, and have reached the present invention.

That is, according to the present invention, in producing a granular nonionic detergent composition containing at least a nonionic surfactant, a washing builder and a fragrance, the nonionic surfactant and the fragrance are mixed in advance, and then the mixture is washed with the fragrance. There is provided a method for producing a granular nonionic detergent composition, which comprises subjecting a builder to stirring granulation or kneading crushing granulation.

[0008]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in detail. The method for producing a granular nonionic detergent composition of the present invention comprises the steps of: (i) mixing a nonionic surfactant and a fragrance in advance when producing a granular nonionic detergent composition containing at least a nonionic surfactant, a washing builder, and a fragrance; A nonionic-perfume mixture is prepared, and b) the mixture and the washing builder are subjected to stirring granulation or kneading crushing granulation.

Heretofore, in producing a granular nonionic detergent composition, a liquid nonionic surfactant has been gradually added or sprayed while mixing the washing builders to obtain a uniform mixture, and then a flavor and other small components are added to the mixture. It was common to add and mix (see JP-A-4-339898). However, when a small amount of a component such as a fragrance is blended into the detergent granule, the fragrance is inevitably deteriorated during long-term storage. However, in the method of the present invention, after preparing the nonion-perfume mixture in the previous reaction step, the mixture and the washing builder are subjected to a granulation step,
A granular nonionic detergent composition capable of maintaining good odor (fragrance) even during long-term storage can be obtained.

In the method of the present invention, various nonionic surfactants can be used as the nonionic surfactant. Preferred nonionic surfactants include, for example, the following.

(1) 6 to 22 carbon atoms, preferably 8 to 1 carbon atoms
Polyoxyalkylene alkyl (or alkenyl) obtained by adding an alkylene oxide having 2 to 4 carbon atoms to an aliphatic alcohol having an average of 3 to 30 mol, preferably 5 to 20 mol.
ether. Among them, polyoxyethylene alkyl (or alkenyl) ether and polyoxyethylene polyoxypropylene alkyl (or alkenyl) ether are preferable. (2) Polyoxyethyl alkyl (or alkenyl) phenyl ether.

(3) Fatty acid alkyl ester alkoxylate represented by the following formula wherein alkylene oxide is added between ester bonds of long-chain fatty acid alkyl ester. R ¹ CO (OA) n OR ² (R ¹ CO represents a fatty acid residue having 6 to 22, preferably 8 to 18 carbon atoms. OA represents a fatty acid residue having 2 to 4 carbon atoms such as ethylene oxide and propylene oxide, preferably Represents an additional unit of alkylene oxide of 2 to 3. n represents an average number of moles of alkylene oxide added, and generally represents 3 to 3;
0, preferably a number from 5 to 20. R ² has 1 carbon atom
Represents a lower alkyl group which may have 1 to 3 substituents. )

(4) Polyoxyethylene sorbitan fatty acid ester. (5) Polyoxyethylene sorbite fatty acid ester. (6) Polyoxyethylene fatty acid esters. (7) Polyoxyethylene hydrogenated castor oil. (8) Glycerin fatty acid ester.

Among the above-mentioned nonionic surfactants, polyoxyethylene alkyl (or alkenyl) ethers having a melting point of 40 ° C. or lower and an HLB of 9 to 16 and fatty acid methyl ester ethoxylate obtained by adding ethylene oxide to fatty acid methyl ester are particularly preferable. Used for Further, these nonionic surfactants may be used as a mixture.

The nonionic surfactant is contained in the granular nonionic detergent composition preferably in an amount of 15 to 50% by weight, more preferably 15 to 40% by weight, and particularly preferably 15 to 35% by weight. If this amount is less than 15% by weight, the resulting detergent particles will have a low nonionic surfactant concentration as well as a low bulk density. The result is contrary to compactness, which is not preferable. It is also not preferable in terms of resource saving. On the other hand, if it exceeds 50% by weight, there is no particular problem in the case of batch-type production, but in the case of continuous production, the amount of adhesion to the granulator increases, and it becomes difficult to produce stably. Is not preferred.

In the practice of the present invention, first, a nonionic surfactant and a fragrance are mixed to prepare a nonion-fragrance mixture, and the following fragrances are used. (1) C10-C15 alcohol (2) C7-C10 aromatic alcohol (3) C8-C17 formate or acetate (4) C10-C15 hydrocarbon (5) Aromatic aldehydes having 7 to 15 carbon atoms (6) Aliphatic aldehydes having 8 to 14 carbon atoms (7) Phenolic fragrance Specific examples of these fragrances include the following compounds.

(1) Alcohol having 10 to 15 carbon atoms: linalool, geraniol, nerol, citronellol,
Dimethyloctanol, hydroxycitronell, tetrahydrolinalool, farnesol, nerolidol,
Santa roll, cedrol, vetiverol, α-terpineol, 1-menthol, borneol, and the like.

(2) Aromatic alcohols having 7 to 10 carbon atoms: benzyl alcohol, β-phenylethyl alcohol, β-phenylpropyl alcohol, cinamic alcohol, dimethylbenzylcarbinol, dimethylphenylcarbinol and the like.

(3) Formate or acetate having 8 to 17 carbon atoms: geranyl formate, benzyl formate, phenylethyl formate, tosilonyl acetate, geranyl acetate, linalyl acetate, bornyl acetate, terpinyl acetate, benzyl acetate, phenylethyl acetate, Phenylpropyl acetate, seryl acetate, -pt-butylcyclohexyl acetate and the like.

(4) Hydrocarbons having 10 to 15 carbon atoms: α-
Pinene, β-pinene, limonene, terpinolene, β-
Cariole frane and the like.

(5) Aromatic aldehyde having 7 to 15 carbon atoms: benzaldehyde, phenylacetaldehyde, cinnamaldehyde, α-amylcinnamaldehyde, α
-Hexylcinnamaldehyde, cyclamenaldehyde, lillyaldehyde and the like.

(6) aliphatic aldehydes having 8 to 14 carbon atoms: n-octyl aldehyde, n-nonyl aldehyde,
n-decylaldehyde, citronellal, citral,
n-undecylaldehyde, undecylenaldehyde,
Dodecyl aldehyde, n-hexadecyl aldehyde and the like.

(7) Phenolic fragrances: thymol, carvacrol, eugenol, isoeugenol and the like.

In the method of the present invention, since a step of preparing a nonionic-fragrance mixture in advance is employed, in the case of producing a granular nonionic detergent composition by a conventional method, alkali builder or water in the detergent is not used. For example, (i) esters of short-chain fatty acids and intramolecular esters (ii) short-chain primary aliphatic aldehydes (iii) phenols such as vanillin Some fragrances can also be used because chemical changes are suppressed.

As such a fragrance, there are 8 to 17 carbon atoms.
And acetic acid esters, aromatic aldehydes having 7 to 15 carbon atoms, aliphatic aldehydes having 8 to 14 carbon atoms, and the compounds exemplified above as phenolic fragrances.

The mixing of the nonionic surfactant and the fragrance in the method of the present invention is carried out at a temperature above the fluidization point of the nonionic surfactant, generally at 20 to 80 ° C, preferably 20 to 60 ° C. Stirring may be such that the mixture is uniformly mixed, and can be allowed to stand still. As a device to be used, a tank provided with a stirring blade is preferable.

The content of the fragrance in the final granular nonionic detergent composition is 0.001 to 1% by weight, preferably 0.01 to 0.8% by weight, and more preferably 0.05 to 1% by weight.
Supplied to be 0.5% by weight.

In the method of the present invention, the nonionic-perfume mixture obtained in the above step and the washing builder are then subjected to stirring granulation or kneading crushing granulation to produce a granular nonionic detergent composition. Note that, in the granular nonionic detergent composition, a small amount of components usually blended in detergents, for example, a fluorescent agent, an enzyme, a bleaching agent, an antistatic agent, a surface modifier, an anionic surfactant, a re-contamination inhibitor, a bulking agent. , A reducing agent and the like may be blended, and these components may be blended in the present granulation step, or may be blended in the detergent particles obtained in the present step.

In the method of the present invention, a builder usually used for detergents is used as a washing builder. For example, chelate builders such as zeolite, tripolyphosphate, citrate, succinate, polyacrylate, acrylic acid-maleic acid copolymer, EDTA,
Alkaline builders such as alkali metal carbonates (such as sodium carbonate and potassium carbonate), alkali metal silicates (such as sodium silicate and potassium silicate), and layered polysilicates (such as macatite and kanemite) are included.

The washing builder is mixed with the nonion-perfume mixture in an amount such that it is generally present in the particulate nonionic detergent composition in an amount of from 20 to 80% by weight, preferably from 30 to 70% by weight, more preferably from 40 to 60% by weight. Granulated. If the amount of the cleaning builder is less than 20% by weight, the detergency is reduced. If the amount is more than 80% by weight, the amount of other components is relatively reduced. For example, the amount of the nonionic surfactant is reduced. It is not preferable because the force decreases.

The following are specific examples of components to be mixed in the detergent. (1) Fluorescent agent: bis (triazinylamino) stilbene disulfonic acid derivative, bis (sulfostyryl) biphenyl salt [Tinopearl CBS] and the like. (2) Enzymes: lipase, protease, cellulase, amylase and the like. (3) Bleaching agents: percarbonates, perborates, etc. (4) Antistatic agents: cationic surfactants such as dialkyl-type quaternary ammonium salts. (5) Surface modifier: fine calcium carbonate, fine zeolite, polyethylene glycol and the like. (6) Anionic surfactant: α-sulfofatty acid methyl ester salt, linear alkylbenzene sulfonate, α-olefin sulfonate, alkyl sulfate, fatty acid soap and the like. (7) Anti-redeposition agent: cellulose derivatives such as carboxymethyl cellulose. (8) Extenders: sodium sulfate, potassium sulfate, sodium hydrochloride and the like. (9) Reducing agents: sodium sulfite, potassium sulfite and the like.

In the method of the present invention, the nonionic
The fragrance mixture and the washing builder are subjected to stirring granulation or kneading crushing granulation to produce a granular nonionic detergent composition.

In the stirring granulation method, as a stirring granulator, a high-speed mixer (manufactured by Fukae Kogyo Co., Ltd.), a sugar mixer (manufactured by Hosokawa Micron Co., Ltd.), a Ledige mixer (manufactured by Matsubo Co., Ltd.) A stirring blade is provided inside the granulator, and the distance between the stirring blade and the inner wall of the granulator is 30 m.
m to the internal stirring type granulator with a clearance of less than
A granular nonionic detergent composition can be produced by introducing and treating a nonionic surfactant and a washing builder, and further optionally addable components.

The temperature of the stirring granulation is generally 20 to 60 ° C.
Preferably 30 to 50 ° C, more preferably 35 to 50 ° C
It is. If the temperature is lower than 20 ° C., granulation is difficult to proceed, which is not preferable. On the other hand, if the temperature is higher than 60 ° C., on the contrary, adhesion to the granulator occurs, and the load tends to be excessive, which is not preferable. In addition, the treatment time in the stirring granulation treatment is usually 1 to 10 minutes, preferably 2 to 8 minutes.
Minutes.

In the kneading crushing granulation method, a nonionic surfactant and a washing builder, and if necessary, a kneading extruder, preferably a closed-type consolidation treatment device, more preferably a horizontal continuous kneader, are added to a kneading extruder. Other optional components are introduced and mixed while imparting shearing force in a kneader to form a granulated product (solid detergent), and then crushed and granulated by a crushing granulator, preferably a cutter mill, and compacted. It can be manufactured by processing. In this case, in addition to the kneader, a single-screw or twin-screw extruder can be used. Specific examples of the kneading extruder used in the present invention include a KRC kneader manufactured by Kurimoto Ironworks Co., Ltd. As the crushing granulator used in the present invention,
For example, Fitzmill [Hosokawa Micron Co., Ltd.
KASO type 6] can be used. During crushing and granulation, for example, crystalline sodium aluminosilicate may be added as a grinding aid.

The temperature of the kneading extruder is generally 30 to 60 ° C., preferably 35 to 55 ° C., more preferably 40 to 50 ° C. If the temperature is lower than 30 ° C., the load on the kneading extruder tends to be excessive, which is not preferable. On the other hand, if the temperature is higher than 60 ° C., on the contrary, the kneaded material tends to adhere to the pulverizer, which is not preferable. Processing time is typically 0.2
２2 minutes, preferably 0.5-1 minute. The crushing and granulation treatment is generally performed at 5 to 30 ° C., preferably 10 to 2 ° C.
The temperature is 5 ° C, more preferably 10 to 20 ° C. Temperature is 5 ℃
If it is lower than the above range, dew condensation easily occurs, which is not preferable. On the other hand, if the temperature is higher than 30 ° C., on the other hand, adhesion to the pulverizer tends to occur, which is not preferable. The processing time is usually 1 to 30 seconds, preferably 3 to 30 seconds.

According to the method of the present invention, the bulk density is 0.3 to 1.2 g / ml, preferably 0.5 to 0.5 g by stirring granulation or kneading crushing granulation using the nonion-flavor mixture.
１1 g / ml consolidation can be obtained. Further, the detergent particles thus produced may be subjected to a coating treatment by adding a coating agent in a rolling drum, for example. Thereby, the flow characteristics can be improved. As the coating agent, an inorganic powder having a passing amount of 50% or more according to a JIS 200 mesh sieve is suitable. For example, carbonates such as sodium carbonate and calcium carbonate, amorphous silica, calcium silicate, and silicate Silicates such as magnesium and aluminosilicates such as zeolite can be used. The coating agent is generally present in the granular nonionic detergent composition of the present invention in an amount of about 0.1%.
It is used in an amount of 5 to 15% by weight, preferably 1 to 10% by weight.

Further, a small amount of a component such as an enzyme can be added to the detergent particles thus produced. The resulting granular nonionic detergent composition generally has an average particle size of 300
3,000 μm, preferably 350-2000 μm, particularly preferably 400-1000 μm.

[0039]

The present invention will be described below in more detail with reference to examples and comparative examples. In the examples and comparative examples, each sample was evaluated by the following test methods.

<Odor test> Coated cardboard (basis weight: 350 g / m ² ), wax sand paper (basis weight: 30) from the outside
g / m ² ) and kraft pulp paper (70 g / m ² ) were used to form a box having a length of 15 cm, a width of 9.3 cm and a height of 18.5 cm. 1.2kg sample in this box
Was stored in a thermo-hygrostat at 45 ° C. and 85% HR for 30 days, and then subjected to a sensory evaluation according to the following criteria. ◎: Odor equivalent to that before storage and good ○: Almost the same odor as before storage and good △: Slightly different odor than before storage but acceptable level ×: Storage An unacceptable level with a noticeable odor compared to before

Example 1 The amounts of the washing builder and amorphous silica (W
C) with a Redigue mixer (Matsubo Corporation, M-2
0 type], and these components were mixed for 30 seconds under stirring with a spindle (200 rpm) and a chopper (6000 rpm). Next, a mixture of the nonionic surfactant and the fragrance (composition of Table 1) in the amounts shown in Table 2 was added, and the average particle size was 5
Granulation was performed until the thickness became 00 μm. Finally, the other optional components [A-type zeolite (CZ), enzyme, sodium percarbonate (PC)] were added in the amounts shown in Table 2 and mixed for 30 seconds to obtain a granular nonionic detergent composition (average particle diameter 500 μm). . Table 2 shows the evaluation results.

Example 2 A mixture of a nonionic surfactant and a fragrance (composition shown in Table 1), a washing builder and WC in the amounts shown in Table 2 below were introduced into a continuous kneader (KRC-4, manufactured by Kurimoto Iron Works Co., Ltd.). After the solid detergent was formed, the solid detergent was mixed with a crushed granulator [DKASO6 type manufactured by Hosokawa Micron Corporation] in the presence of fine A-type zeolite powder (CZ) in the amount shown in Table 2 to obtain an average particle size. Granulation was performed until the particle size became 500 μm. Finally, other optional components (CZ, enzyme, PC) were added in the amounts shown in Table 2 to obtain a granular nonionic detergent composition (average particle size: 500 μm). Table 2 shows the evaluation results.

Comparative Example 1 The washing builder and WC in the amounts shown in Table 2 below were charged into a Lodige mixer [M-20, manufactured by Matsubo Co., Ltd.], and the main spindle (200 rpm) and the chopper (6000 rpm) were stirred. For 30 seconds. Then, Table 2
Was added and granulated until the average particle diameter became 500 μm. Finally, the perfume (composition of Table 1) and other optional components (CZ, enzyme, PC) were added in the amounts shown in Table 2 and mixed for 30 seconds to obtain a granular nonionic detergent composition (average particle diameter 500 μm). Table 2 shows the evaluation results.

<Raw Materials> The nonionic surfactants, cleaning builders and fragrances used in Examples and Comparative Examples were
It is as follows.

A) Nonionic surfactant C ₁₂ H ₂₅ O (CH ₂ CH ₂ O) ₆ H [Polyoxyethylene alkyl ether obtained by adding an average of 6 moles of ethylene oxide to Conol 20P manufactured by Shin Nippon Rika Co., Ltd.] Builder (1) Cleaning builder A zeolite A [Silton B manufactured by Mizusawa Chemical Co., Ltd.] (2) Cleaning builder B layered silicate [SKS-6 manufactured by Hoechst] (3) Cleaning builder C Light sodium carbonate [Asahi Glass Co., Ltd.] Light ash) c) Fragrance Composition shown in Table 1

[0046]

[Table 1] Component content (parts by weight) ────────────────────────────────── 3,7- Dimethyl-1,6-octadien-3-ol 80 3,7-dimethyl-1,6-octadien-3-yl-acetate 60 3,7-dimethyl-6-octen-1-ol 40 β-phenylethyl alcohol 50 p-tert-butyl-α-methylhydrocinnamic aldehyde 70 α-methyl-p-isopropylphenylpropionaldehyde 60 α-n-amylcinnamic aldehyde 20 α-n-hexylcinnamic aldehyde 60 7-acetyl-1,1 , 3,4,4,6-hexamethyltetrahydronaphthalene 80 3- (5,5,6-trimethyl-norbalnan-2-yl) cyclohexane-1-o Reference Signs List 20 belt fix 30 2-ethyl-4- (2,2,3-trimethyl-3-cyclopent-1-yl) -2-butan-1-ol 10% 10 α, α-dimethyl-p-ethylhydrocinamic Aldehyde 40 2,4-dimethyl-3-cyclohexene-1-carboxaldehyde 10 cis-3-hexenol 10 2-trans-3,7-dimethyl-2,6-octadien-1-ol 30 n-decylaldehyde 5 10- Undecene-1-al 5 methylnonylacetaldehyde 5 4- (4-hydroxy-4-methylpentyl) -3-cyclohexene-1-carboxaldehyde 30 naphthalene-2-acetyl-1,2,3,4,6,7, 8-octahydro-2,3,8,8-tetramethyl 30 5- (2-methylene-6 , 6-Dimethyl-cyclohexyl) -4-pentan-3-one 50 2-methoxy-4-propenylphenol 20 allylcyclohexanepropionate 10 6,7-dihydro-1,1,2,3,3-pentamethyl-4 (5H) -Indanone 5 p-Propenylphenyl methyl ether 5 Methyl-2-aminobenzoate 5 Lemon oil 30 Orange oil 20 Lavandin oil 20 Patchouli oil 10 3,7-Dimethyl-2,6-octadienal 30 Methyldihydrojasmo Nate 50 Percentage of perfume components having a boiling point of 230 ° C. (1 atm) in the total perfume (wt%) 66

[0047]

[Table 2] Note) Enzyme: mixture of lipase / protease / cellulase = 1/1/1 PC: sodium percarbonate (manufactured by Mitsubishi Chemical Corporation) CZ: zeolite A [Silton B manufactured by Mizusawa Chemical Co., Ltd.] WC: amorphous silica [ Tokusyl N manufactured by Tokuyama Corporation]

From the results shown in Table 2, it can be seen that the granular nonionic detergent composition obtained by the method of the present invention can retain a good odor even after storage for 4 weeks.

[0049]

According to the method of the present invention, in producing a granular nonionic detergent composition containing at least a nonionic surfactant, a washing builder and a fragrance, the nonionic surfactant and the fragrance are mixed in advance, and then the mixture is mixed. By subjecting the washing builder and the washing builder to stirring granulation or kneading crushing granulation, it is possible to suppress the deterioration of the fragrance even after long-term storage and obtain a granular nonionic detergent composition capable of maintaining a good odor (fragrance). .

Claims (1)

[Claims] In producing a granular nonionic detergent composition containing at least a nonionic surfactant, a cleaning builder and a fragrance, the nonionic surfactant and the fragrance are mixed in advance, and then the mixture and the cleaning builder are agitated or granulated. A method for producing a granular nonionic detergent composition, comprising kneading and crushing and granulating.