JP2000239692A - Perfume particle composition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a perfume particle composition which, when mixed into a particulate detergent, gives a particulate detergent composition having an optimal strength of perfume and improves the perfume during cleaning and the perfume remaining on clothes after cleaning by incorporating a perfume component, a surfactant, oil-absorbing particles, a water-soluble polymer, and water into the same. SOLUTION: This perfume particle composition contains (A) 1-20 wt.% perfume component, (B) 10-94 wt.% surfactant comprising an anionic surfactant and/or a nonionic surfactant, (C) 1-60 wt.% at least one kind of particles selected from among white carbon and amorphous aluminosilicates and exhibiting an oil absorption (JIS K 6220) of 100-800 ml/100 g, (D) 1-20 wt.% water-soluble polymer in a wt. ratio of B/D of 5-50, and (E) 0.1-20 wt.% water. Preferably, the perfume particle composition has a particle size of 100-3,000 μm, and 0.1-50 wt.% perfume particle composition is formulated in the final detergent composition.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a fragrance particle composition used for a granular detergent or the like.

[0002]

2. Description of the Related Art
A fragrance is blended for the purpose of masking and scenting odors derived from the detergent composition, and scenting clothes after washing. However, high-density granular concentrated detergents have a high density and have a high content of active ingredients such as surfactants, and have reduced the amount used per wash. When the fragrance is applied, the amount of the fragrance component used in the washing liquid and the laundry is reduced, and the scent of the washing liquid and the residual scent on the washed clothes are inferior. On the other hand, if the fragrance rate for the detergent is increased in order to compensate for this defect, the scent of the powder becomes strong and unpleasant. In addition, a perfume component that deteriorates by directly perfuming the detergent cannot be used.

Japanese Patent Application Laid-Open No. Hei 10-53791 discloses a fragrance particle comprising a water-insoluble solid particle having an anionic surfactant and water of crystallization and having an average particle diameter of 20 μm or less. Further improvements are desired.

[0004]

The present invention comprises the following component (a):
(E) a perfume particle composition, and a granular detergent containing the perfume particle composition. (a) Perfume ingredient 1 to 20% by weight (b) Surfactant 10 to 94% by weight (c) Oil absorption capacity measured based on JIS K6220 is 100 to 800ml
1/60% by weight of particles / 100g (d) 1-20% by weight of water-soluble polymer [However, component (b) and component
The weight ratio of (d) is (b) :( d) = 5: 1 to 50: 1. (E) water 0.1 to 20% by weight Further, the present invention, after mixing the above component (a) and component (c),
There is provided a method for producing the above-mentioned perfume particle composition, in which other components are mixed.

[0005]

BEST MODE FOR CARRYING OUT THE INVENTION <Component (a)>
For example, "Patent Office Bulletin 10 (1998) -25 [7159] Well-known and commonly used techniques (powder detergent for clothing)" (Japan Patent Office, 1998
Ingredients described on page 42, bottom line 4, line 45 to page 45, line 244, or "Chemistry of Perfume in the Industrial Chemistry Series" (edited by The Chemical Society of Japan, Ryoichi Akahoshi, Dainippon) Perfume components described in Tosho Co., Ltd., issued on September 16, 1983) can be used. In particular, the fragrance itself is too strong, but the fragrance particles of the present invention give an appropriate odor. In view of giving an appropriate odor, aldehydes, esters, lactones, phenol compounds, hydrocarbons containing one or more double bonds in the molecule or It preferably contains at least one compound selected from the group consisting of alcohols, ethers or ketones, organic compounds containing nitrogen or sulfur, and synthetic musks.

Examples of the aldehyde include aliphatic aldehydes such as heptyl aldehyde, decyl aldehyde, undecyl aldehyde, dodecyl aldehyde, methyl nonyl acetaldehyde, undecylenaldehyde and the like; citral,
Terpene aldehydes such as hydroxycitronellal, citronellal and perilaldehyde; aromatic aldehydes such as benzaldehyde, α-hexylcinnamic aldehyde, lilial, heliotropin, vanillin, ethyl vanillin, cuminaldehyde; And other aldehydes.

As esters, ethyl formate, benzyl formate, linalyl formate, citronellyl acetate, butyl acetate,
Linalyl acetate, isononyl acetate, geranyl acetate, terpinyl acetate, isobornyl acetate, tricyclodecenyl acetate, benzyl acetate, phenylethyl acetate, styralyl acetate, cinnamyl acetate, hexyl acetate, acetyl eugenol, acetyl isoeugenol, ceryl acetate, ot-
BCHA, hexyl salicylate, benzyl salicylate,
Fruitate and the like can be mentioned.

[0008] As the lactone, γ-octalactone,
γ-nonalactone, σ-decalactone, γ-undecalactone, coumarin and the like.

The phenolic compounds include eugenol, isoeugenol, thymol and the like.

Examples of the hydrocarbon containing one or more double bonds in the molecule include limonene, dipentene, terpinolene, α-
Pinene, β-pinene, p-cymene and the like.

The alcohol containing one or more double bonds in the molecule includes cis-3-hexenol, santalol,
Linalool, geraniol, citronellol, dihydromyrcenol, phenylethyl alcohol, dimethylbenzylcarbinol and the like.

Examples of the ether having one or more double bonds in the molecule include nerol oxide, rose oxide, linalool oxide and the like.

Examples of the ketone containing one or more double bonds in the molecule include ionone, methylionone gamma, damascon, damacenone, dynascon, maltol, iso-e-super, and the like.

Examples of the nitrogen-containing or sulfur-containing organic compound include indole, skatole, citronellyl nitrile,
Geranyl nitrile and the like can be mentioned.

Synthetic musks include ethylene brassate, cyclopentadecanolide, Pearlide
And the like.

It is also possible to use other flavor components in combination. The content of the component (a) is 1 to 20% by weight, preferably 1 to 12% by weight in the composition in view of the strength of the scent, fluidity and handling properties.

<Component (b)> As the surfactant used in the present invention, an anionic surfactant and / or a nonionic surfactant are preferable, and fatty acid salts, alcohol sulfate salts, alkyl ether sulfate salts, and sulfuric acid salts are preferred. Olefin, alkylbenzene sulfonate, α-olefin sulfonate, alcohol alkylene oxide (eg, ethylene oxide) adduct, fatty acid monoglyceride,
Examples include fatty acid diglyceride, pentaerythritol fatty acid monoester, sorbitan fatty acid monoester, sucrose fatty acid monoester, fatty acid alkanolamide and the like. In particular, those represented by the following formula (I) are preferable from the viewpoint of proper granulation. R-OSO ₃ Na (I) wherein R represents a hydrocarbon group having 6 to 20 carbon atoms. ].

In the present invention, salts of sulfates of primary alcohols having a hydrocarbon group such as an alkyl group or an alkenyl group having 6 to 18, particularly 10 to 18 carbon atoms and having an iodine value of 5 or less are more preferable. Specific examples include sodium salts such as decyl sulfate, lauryl sulfate, myristyl sulfate, cetyl sulfate, and stearyl sulfate.

The content of the component (b) is from 10 to 94% by weight, preferably from 40 to 94% by weight in the composition in view of the stability of the perfume particle composition.
% By weight, more preferably 50 to 94% by weight, particularly preferably
60-94% by weight.

<Component (c)> The particles used in the present invention include:
From the standpoint of preventing the perfume particle composition from becoming fine particles, and having fluidity and handling properties, the oil absorption capacity measured based on JIS K6220 is 100 to 800 ml / 100 g, preferably 150 to 600 ml / 100 g. Further, by containing the component (c), the contact of the flavor component with the detergent composition is reduced, so that the storage stability can be greatly improved. In particular, it is advantageous for a fragrance component which could not be used conventionally.

As the component (c), there can be mentioned particles composed of at least one selected from white carbon and amorphous aluminosilicate. Here, white carbon refers to hydrous finely divided silica, calcium silicate, hydrous silicon dioxide and mixtures thereof.

As an example of the component (c), JP-A-62-191417, page 2, lower right column, line 19 to page 5, upper left column, line 17 (particularly the initial temperature is in the range of 15 to 60 ° C.) Preferred), JP-A-62-191.
No. 419, page 2, lower right column, line 20 to page 5, upper left column, line 11 (in particular, the oil absorption is preferably 170 mL / 100 g), and JP-A-9-132794. Column 17, line 46 to column 18, line 38, JP-A-7-10526, column 3, line 3 to column 5, line 9, JP-A-6-227811, column 2, line 15
Amorphous aluminosilicates (oil absorption capacity 285 mL / 100 g) described in lines from line 5 to column 2, line 2 and column 2 line 18 to column 3 line 47 in JP-A-8-119622, etc. Can be. For example, Toksil NR (manufactured by Tokuyama Soda Co., Ltd .: Oil absorption capacity 210)
~ 270mL / 100g), Fluorite (same: oil absorption capacity 400 ~ 600mL)
/ 100g), TIXOLEX 25 (manufactured by Han France Chemical Co., Ltd .: 220-270m oil absorption capacity)
L / 100 g) or Silopure (Fuji Divison Co., Ltd .: oil absorption capacity 240 to 280 mL / 100 g). Particularly, as the oil-absorbing carrier, JP-A-5-5100, column 4, line 34 to column 6, line 16 (particularly, an oil-absorbing carrier in column 4, lines 43 to 49) and JP-A-6-79899, 12 Column 12th row-Column 13th
Those having the properties described in line 17, line 17, column 17, line 34 to column 19, line 17 are preferred. Among them, those having a peak pore diameter of 0.1 to 10 μm by a mercury intrusion method are preferable. The shape is not particularly limited.

The content of the component (c) is from 1 to 60% by weight in the composition in view of retention of the fragrance component, fluidity of the fragrance particle composition, handleability, and solubility of the fragrance particle composition during washing. , Preferably 3 to 50% by weight, more preferably 3 to 40% by weight,
Particularly preferably, it is 3 to 30% by weight.

<Component (d)> The water-soluble polymer used in the present invention includes polyacrylic acid or a salt thereof, polyethylene glycol, an acrylic acid-maleic acid copolymer or a salt thereof, starch, cellulose, polyvinylpyrrolidone and Mixtures thereof are mentioned, and each polymer has an average molecular weight of 3,000 to 100,000. Particularly, polyethylene glycol, an acrylic acid-maleic acid copolymer or a salt thereof, and polyvinylpyrrolidone are preferable.

The content of the component (d) is from 1 to 20% by weight, preferably from 1 to 20% by weight, in view of maintaining the strength of the perfume particle composition, preventing undesired fine particles, and stabilizing the odor after storage. ~
10% by weight. Also, the weight ratio of component (b) to component (d) is
In terms of maintaining strength and fluidity of the perfume particle composition, (b) :( d) =
5: 1 to 50: 1, more preferably 10: 1 to 40: 1.

The content of water (e) is from 0.1 to 20% by weight, preferably from 1 to 15% by weight, particularly preferably from 1 to 15% by weight in the composition, in order to reduce odor dispersion by storage and prevent odor deterioration. 10% by weight. The water content can be determined, for example, by the NMR method.

The perfume particle composition of the present invention may contain known dyes, pigments, fluorescent dyes and inorganic salts such as sodium sulfate, sulfite, carbonate, tripolyphosphate and silicate.

Also, especially for the aesthetic appearance when the perfume particle composition of the present invention is dry-mixed with the granular detergent composition, CIAc
id Red 52 (CI 45110); for example, Red No. 106, CI
AcidBlue 9 (CI 42090); As an example, Blue No. 1, CI
Acid Yellow 3 (CI 47005); for example, a dye such as Yellow No. 203 or CI Pigment Green 7 (CI 74260); for example, Lionol Green FB, CI Pigment Blue 15 (CI 741)
60); As an example, it is desirable to add a pigment such as Cyanine Blue BR to the fragrance particle composition of the present invention.
It is desirable to add pigments such as 4260 and CI 74160.

The particle size of the perfume particle composition of the present invention is preferably from 100 to 300 in terms of perfume release and particle solubility.
0 μm, more preferably 300 to 1500 μm, particularly preferably
It is 500-1500 μm.

The fragrance particle composition of the present invention is preferably prepared by mixing the above components (a) and (c), and then mixing the components (b) and (d).
And another component such as component (e).

The fragrance particle composition of the present invention is incorporated in the final detergent composition in an amount of 0.1 to 50% by weight, particularly 0.2 to 30% by weight. As the granular detergent to which the fragrance particle composition of the present invention is mixed, for example, dry-mixed, a conventionally known detergent composition can be used, but the composition may contain a fragrance component. The granular detergent having a high bulk density is suitable, and the final bulk density after blending the perfume particle composition is adjusted to 0.6 to 1.2 g / cm ³ . Further, the fragrance particle composition of the present invention can be blended with a solid detergent, a paste-like detergent, a bleaching agent composition, a softening agent composition and the like.

[0032]

EXAMPLES Examples (I) to (IV) and Comparative Examples (I) to (II) (1) Perfume particle composition The following production examples were prepared using the perfume component (i) and the various components shown in Tables 1 and 2. A fragrance particle composition was prepared according to (i) or (ii).
Here, the composition of the flavor component (i) is hexyl salicylate 2
0%, linalool 20%, γ-undecalactone 5%, IsoE Super 10%, benzyl acetate 20%, eugenol 5%, furtate 15%, vanillin 5% (all by weight).

Production Example (i) Production Example (i) of the fragrance particle composition is shown below by taking Example (I) as an example.

100 kg of Tixosil 38 (Cofran) is put into an R-shaped ribbon mixer, and 25 kg of the fragrance component (i) is dropped into the mixer over 5 minutes while rotating the mixer at 20 rpm, and then for 15 minutes Rotate, add 350 kg of sodium lauryl sulfate (Emal 10P manufactured by Kao Corporation), rotate for 15 minutes, mix 10 kg of polyethylene glycol (average molecular weight 6000) and 15 kg of water, and melt at 60 ° C. Drip into the mixer and spin for another 15 minutes. The powder thus obtained was subjected to extrusion granulation, sieving, and further sieving through a 500 μm sieve to obtain a sample on the sieve.

The compositions of Examples (II), (III) and (IV) were similarly prepared. However, the "other" component was added to the mixer simultaneously with the sodium lauryl sulfate (b).

Production Example (ii) Production Example (ii) of the perfume particle composition is shown below using Comparative Example (I) as an example.

In an R type ribbon mixer, 4A type zeolite
75 kg and 375 kg of sodium lauryl sulfate (Emal 10P manufactured by Kao Corporation) are charged, and after rotating the mixer at 20 rpm for 30 minutes, 25 kg of the perfume ingredient (i) is added to the mixer.
And then rotated for 15 minutes to obtain acrylic acid-maleic acid copolymer (manufactured by BASF, Sokalan CP-5).
A mixture of 15 kg of water and 15 kg of water was melted at 60 ° C., dropped into a mixer, and further rotated for 15 minutes. The powder thus obtained was subjected to extrusion granulation, sieving, and further sieving through a 500 μm sieve to obtain a sample on the sieve. The composition of Comparative Example (II) was similarly prepared.

(2) Powder Synthetic Detergent A or B <Powder Synthetic Detergent A> 1.0 kg of 4A type zeolite, sodium linear alkyl (C ₁₂ ) benzenesulfonate (hereinafter, LAS)
4.0kg, polyoxyethylene primary dodecyl ether (HLB
= 13.1, hereinafter, AE) 0.3 kg, acrylic acid-maleic acid copolymer (manufactured by BASF, Sokaran CP-5, hereinafter, AA-MA copolymer) 0.5 kg, carboxymethyl cellulose 0.15 kg,
Sodium tallow fatty acid (hereinafter FA) 0.1kg, JIS No. 2 sodium silicate 1.0kg, soda ash 0.5kg and fluorescent dye (4,4'-bis- (2-sulfostyryl) biphenyl salt) 0.05kg to 60%
A solid water slurry is obtained, and the particles obtained by spray-drying the slurry are put into a Loedige mixer.
1.0 kg, 0.5 kg of soda ash, 0.1 kg of enzyme [3: 1: 1 mixture of lipolase 100T, cellzyme 0.1T, termamyl 60T (all manufactured by Novo Nordisk)], and sodium sulfate used for balance are added and mixed. In the process, 0.2 kg of AE heated to 70 ° C. was gradually dropped to perform granulation. Further, 0.25 kg of 4A type zeolite was added and granulated, and a powder synthetic detergent A was obtained except for those not passing through a 1410 μm sieve (mean particle size: 45).
0 μm, bulk density 750 g / L).

<Powder Synthetic Detergent B> Sodium Tripolyphosphate
1.5 kg, LAS 4.0 kg, AE 0.3 kg, AA-MA copolymer 0.1 kg,
Carboxymethylcellulose 0.05kg, FA 0.1kg, JIS 2
No.1 sodium silicate 1.0kg, soda ash 0.2kg and fluorescent dye 0.05kg
Was obtained in the same manner as in the case of the above-mentioned powdery synthetic detergent A except that a water slurry having a solid content of 50% was obtained (average particle size: 400 μm, bulk density: 700 g / L).

(3) Perfume particle-containing powder detergent 5% by weight of the perfume particle composition obtained in the above (1) is mixed with the powdery synthetic detergent A or B obtained in the above (2), and the perfume particle-containing powder is mixed. A detergent was obtained.

(4) Performance evaluation The powder detergent containing fragrance particles obtained in the above (3) was
The change of scent before and after storage was evaluated by three skilled panelists. The change in fragrance is determined by adding 150 ml of powder detergent or 150 ml of powder detergent before storage to a thimble filter (Advantech Toyo Co., Ltd. No.8
4,40mm x 150mm) and stored for 30 days at 30 ℃ 65% RH, using powder detergent, the strength and taste of the aroma of the grains,
The evaluation was made based on the intensity of the scent when the washing process was performed under the following conditions (the evaluation value is an average value of three persons). The results are shown in Tables 1 and 2.

<Evaluation of powder scent> +: Same scent intensity as control product 0: Slight scent intensity slightly lower than control product A: Scent better than control product B: Control The taste of the fragrance is equal to that of the control product. C: The fragrance is not preferable to the control product.

<Washing conditions> Put 1.5 kg of cloth and 30 L of water into a washing machine, and add 25 g of perfume particle-containing powder detergent before or after storage.
After the mixture was stirred for 15 minutes, it was rinsed twice and evaluated.

On the other hand, as a control product, a powder detergent was prepared by spraying a fragrance onto a powder detergent (containing no fragrance particles) so that the amount of the fragrance in each example was blended. Cylindrical filter paper (Advantech Toyo Co., Ltd. No. 84, 40 mm × 150 mm) was filled with 150 ml of the detergent, and powder detergents after storing at 30 ° C. and 65% RH for 30 days were prepared. Using this control product, a washing treatment was performed under the above conditions, and the result was used as a reference for a change in aroma.

<Evaluation of aroma during washing> A: Intensity of washing water after 1 minute of stirring under the above conditions b: Aroma intensity of washing water after 15 minutes of stirring under the above conditions C: Under the above conditions The intensity of the scent of the dehydrated cloth after stirring and rinsing for 15 minutes The intensity of each scent in the washing process of the above (a) to (c) was evaluated based on the following criteria in comparison with the control product. 3: Very strong fragrance compared to control product 2: Strong fragrance compared to control product 1: Same fragrance as control product

[0046]

[Table 1]

[0047]

[Table 2]

(Note) * 1 Amorphous aluminosilicate: Al ₂ O ₃ / SiO ₂ / Na ₂ O = 2
9.6 / 52.4 / 18.0 (weight ratio), average particle diameter 10 μm, oil absorption capacity 258 ml / 100 g * 2 4A type zeolite; average particle diameter 4 μm (crystal water 20
%) * 3 PEG: average molecular weight 6000 * 4 Dye A: Lionol Green FB [CIPigment Green 7,
(CI 74260)] * 5 Polyvinylpyrrolidone: average molecular weight 30,000 * 6 Dye B: Red No. 106 [CIAcid Red52 (CI 4511)
0)]

[0049]

The fragrance particle composition of the present invention is mixed with a particulate detergent to optimize the intensity of the fragrance of the particulate detergent composition, and to reduce the fragrance during washing and the residual fragrance of clothes after washing. Can be improved. Moreover, the granular detergent composition containing the perfume particle composition of the present invention has good fragrance stability even after storage.

Continued on the front page (72) Inventor Ryuji Yoshida 1334, Minato, Wakayama-shi, Wakayama Prefecture Inside Kao Corporation Research Institute (72) Inventor Tamaki Suzuki 1334, Minato, Wakayama-shi, Wakayama Prefecture Research Institute F-term (reference) 4H003 AB03 AB19 AB27 AC08 BA09 DA01 EA12 EA15 EA16 EA25 EA28 EB28 EB32 EB36 EB42 EC01 ED02 FA26 4H059 AA04 AA11 BA02 BA14 BA17 BA18 BA19 BA20 BA23 BA30 BA35 BA36 BA43 BA44 BB02 BB03 BB18 BB13 BB18 BB13 BB13 BB13 BB13 BB13 BB18 EA11 EA31

Claims (7)

[Claims] 1. A fragrance particle composition comprising the following components (a) to (e): (a) Perfume ingredient 1 to 20% by weight (b) Surfactant 10 to 94% by weight (c) Oil absorption capacity measured based on JIS K6220 is 100 to 800ml
1/60% by weight of particles / 100g (d) 1-20% by weight of water-soluble polymer [However, component (b) and component
The weight ratio of (d) is (b) :( d) = 5: 1 to 50: 1. (E) water 0.1-20% by weight 2. Component (a) is an aldehyde, ester, lactone, phenolic compound, hydrocarbon or alcohol or ether or ketone containing at least one double bond in the molecule, nitrogen-containing or sulfur-containing organic compound, and 2. The fragrance particle composition according to claim 1, comprising one or more compounds selected from the group consisting of synthetic musks. 3. Component (b) is an anionic surfactant and / or
3. The fragrance particle composition according to claim 1, which is a nonionic surfactant. 4. The fragrance particle composition according to claim 1, wherein the component (b) is an anionic surfactant represented by the following formula (I). R-OSO ₃ Na (I) wherein R represents a hydrocarbon group having 6 to 20 carbon atoms. ] 5. The fragrance particle composition according to claim 1, wherein the component (c) is at least one selected from white carbon and amorphous aluminosilicate. 6. A granular detergent containing the fragrance particle composition according to any one of claims 1 to 5. 7. The method for producing a fragrance particle composition according to claim 1, wherein after the component (a) and the component (c) are mixed, other components are mixed.