JPH0255480B2 - - Google Patents

Description

[Detailed description of the invention]

INDUSTRIAL APPLICATION FIELD OF THE INVENTION This invention relates to dense granular concentrated detergent compositions, and more particularly to dense granular concentrated detergent compositions that provide a consumer-desirable fragrance. [Prior Art] In recent years, demand for high-density concentrated powder detergents has been increasing from the viewpoint of resource conservation, transportation of detergents, and convenience for housewives in carrying and storing detergents. As high-density powder detergents, JP-A-48-61511, JP-A-53-36508, JP-A-58-
132093, etc., but all of them relate to the general composition, manufacturing method, or solubility improvement of high-density powder detergents, and none concern the problem of fragrance of high-density powder detergents. [Problem to be solved by the invention] It is common practice to add a specific amount of fragrance to detergent, which masks the raw odor of detergent and makes it suitable for powder, laundry liquid, and washed clothes. This is necessary to impart a unique fragrance and increase product value. However, high-density granular concentrated detergents (high-density here refers to those with a bulk specific gravity of 0.5 g/cm ³ or more) are
Compared to conventional low-density detergents (with a bulk specific gravity of about 0.3 g/ ^cm3 ), the content of active ingredients such as surfactants is increased, and the density is increased to reduce the amount used per wash (weight and (e.g. 40
(from 25 g/30 to 25 g/30). Therefore, when scented at the same rate as conventional low-density detergents, the amount of fragrance ingredients in the washing liquid and laundry decreases according to the amount used, and the scent of the washing liquid increases. Another problem was that the scent remained on washed clothes was too weak. In order to compensate for this drawback, it would be easy to think of increasing the percentage of perfume added to the detergent, but this would cause the problem that the scent of the detergent powder itself would become too strong, causing discomfort. . [Means for Solving the Problems] The present inventors have carried out extensive studies to solve these problems, and have found that by using a specific fragrance composition, it is possible to achieve a high level of fragrance without increasing the percentage of fragrance. The inventors have discovered that it is possible to appropriately control the residual fragrance of dense granular concentrated detergent powder, washing liquid, and washed clothes, leading to the completion of the present invention. That is, in the present invention, a fragrance component with a vapor pressure of 5 to 50 μHg is used.
A fragrance composition comprising 50 to 90% by weight, 40% by weight or less of fragrance components exceeding 50μHg, and 20% by weight or less of fragrance components less than 5μHg, and having a vapor pressure of 5 to 5% by weight.
A high-density granular concentrate characterized by blending a fragrance composition containing 20% by weight or more of one or more fragrance ingredients selected from the group consisting of (1) to (11) below in 50 μHg of fragrance ingredients. A detergent composition is provided. (1) Dimethylbenzyl carbinyl acetate (2) Tricyclo[5.2.1.0 ^2.6 ]-dec-3-ene-
8-yl acetate (3) tricyclo[5.2.1.0 ^2.6 ]-dec-3-ene-
8-ylpropionate (4) 3-amyl-4-acetoxytetrahydropyran (5) 4-tert-butylcyclohexyl acetate (6) 2-tert-butylcyclohexyl acetate (7) p-tert-butyl-α-methyl Hydrocinnamic aldehyde (8) 4-(4-hydroxy-4-methylpentyl)
-3-Cyclohexene-1-carboxaldehyde (9) α-hexylcinnamic aldehyde (10) α-amyl cinnamic aldehyde (11) α,α-dimethyl-p-ethylhydrocinnamic aldehyde What does vapor pressure mean in the present invention? Vapor pressure at 25℃. Examples of fragrance components with a vapor pressure of 5 to 50 μHg include (1) dimethylbenzyl carbinyl acetate (2) tricyclo[5.2.1.0 ^2.6 ]-dec-3-ene-
8-yl acetate (3) tricyclo[5.2.1.0 ^2.6 ]-dec-3-ene-
8-ylpropionate (4) 3-amyl-4-acetoxytetrahydropyran (5) 4-tert-butylcyclohexyl acetate (6) 2-tert-butylcyclohexyl acetate (7) p-tert-butyl-α-methyl Hydrocinnamic aldehyde (8) 4-(4-hydroxy-4-methylpentyl)
-3-Cyclohexene-1-carboxaldehyde (9) α-hexylcinnamic aldehyde (10) α-amyl cinnamic aldehyde (11) α,α-dimethyl-p-ethylhydrocinnamic aldehyde (12) 3,7- Examples include dimethyl-6-octen-1-ol (13) phenylethyl alcohol (14) diphenylamine oxide. Fragrance ingredients with a vapor pressure of 5 to 50μHg are included in mixed fragrances.
50 to 90% by weight (hereinafter abbreviated as %), preferably 50 to 90% by weight
Contains 80%. The perfume component having a vapor pressure of 5 to 50 μHg must contain 20% or more of one or more perfume components selected from (1) to (11) among the above-mentioned perfume components. By blending these specific ingredients, the fragrance retention on clothing is improved. Although the details of the reason are unknown, it is probably due to its affinity with fibers, based on the chemical structure of the fragrance. Perfume ingredients with a vapor pressure exceeding 50 μHg include p
-mentha-1,8-diene, 2-methyl-6-methylene-7-octan-2-ol, 3,7-dimethyl-1,6-octadien-3-ol, p
-menth-1-en-8-yl acetate and the like are exemplified. Flavor ingredients with a vapor pressure of less than 5 μHg include 1, 3,
4,6,7,8-hexahydro-4,6,6,
Examples include 7,8,8-hexamethylcyclopenta-γ-benzopyran, acetylcedrene, cedar wood oil, synthetic sangur, and benzyl benzoate. Fragrance ingredients with vapor pressure exceeding 50 μHg are 0 to 40
%, preferably 25-40%, perfume ingredients less than 5 μHg are incorporated into the perfume composition at 0-20%, preferably 5-20%. There are no particular limitations on the method for producing concentrated powder detergent, but for example, the method disclosed in the above-mentioned Japanese Patent Application Laid-Open No. 48-61511,
As shown in Japanese Patent Application Laid-open No. 53-36508, there is a method in which an alkali agent and an acid-resistant detergent component are added to an unneutralized anionic surfactant, and after neutralization, zeolite, tripoly, etc. are added and crushed. It can be manufactured by a method of increasing the bulk density by granulating a powdered detergent by spray drying. Bulk density is 0.5g/ ^cm3 or more, preferably 0.5-1.5
g/cm ³ , particularly preferably 0.5 to 1.2 g/cm ³ , and even more preferably 0.7 to 1.2 g/cm ³ . The particle size of concentrated powder detergent is preferably 2000μ or less,
More preferably 3% or less is 2000μ or less and 125μ or less, even more preferably 1% is 2000μ or less and 125μ or less
The following are desirable. Furthermore, the composition of the present invention may contain the following commonly used detergent ingredients as required. (1) Alkylbenzene sulfonic acids, alkyl or alkenyl ether sulfates, alkyl or alkenyl sulfates, olefin sulfonates, alkanesulfonates, saturated or unsaturated fatty acid salts,
Anionic surfactants such as α-sulfo fatty acid salts or esters, carboxylic acid salts of alkyl or alkenyl ethers (the content of anionic surfactants is usually in the range of 25-50%, preferably 30-40%) (2) Polyoxyalkylene alkyl or alkenyl ether, polyoxyethylene alkyl phenyl ether, higher fatty acid alkanolamide or its alkylene oxide adduct, sucrose fatty acid ester, fatty acid glycerin monoester, alkylamine oxide (3) Betaine type Surfactants such as amphoteric surfactants, sulfonic acid type amphoteric surfactants, phosphate ester type surfactants, and cationic surfactants (4) Alkali agents such as silicates, carbonates, and sesquicarbonates (5) Zeolite (aluminosilicate), orthophosphate, pyrophosphate, tripolyphosphate, nitrilotriacetate, ethylenediaminetetraacetate,
Divalent metal ion scavengers such as citrate, isocitrate, polyacrylic acid, and polyacetal carboxylic acid (6) Recontamination inhibitors such as polyvinyl alcohol, polyvinylpyrrolidone, carboxymethyl cellulose, and polyethylene glycol (7) Sodium percarbonate, Bleaching agents such as sodium perborate and sodium sulfate hydrogen peroxide adducts (8) Enzymes such as proteases, esterases, lipases, and cellulases (9) Other anticaking agents, bleach activators, peroxide stabilizers, Ingredients commonly used in detergents such as antioxidants, fluorescent dyes, blue tints, photoactivated bleaches, and fragrances [Examples] The present invention will be further described in detail with reference to Examples. The present invention is not limited to the following examples. Example 1 and Comparative Examples 1 to 4 Low-density detergents and high-density granular concentrated detergents with the formulations shown in Table 1 were manufactured, and the scent of the detergent powder and the scent of the washing liquid were scented with the fragrance compositions shown in Table 2. Table 3 shows the results of a comparative study in terms of fragrance and fragrance retention on washed clothes.

【table】

[Table] Each component in Table 1 indicates the following. LAS: Linear alkylbenzene sulfonate sodium (C ₁₂ - C ₁₃ ) AOS: α-olefin sodium sulfonate (C ₁₆ -
C ₁₈ ) Soap; Beef tallow soap (C ₁₆ to _{C 18} ) Nonionic; Polyoxyethylene alkyl ether (C ₁₂ to _{C 13} , = 10) Polyethylene glycol; Average molecular weight approximately 13,000 Small amounts of additives; Fluorescent dyes, enzymes, etc. Table Composition 2 contains 1.6 times the amount of each component other than sodium sulfate compared to Composition 1 of 1.
If the weight used is 1/1.6 of Composition 1, the concentration of each component will be the same as in Composition 1. This is a so-called concentrated composition. Next, Table 2 shows the fragrance ingredients used.

【table】

[Table] The manufacturing method of low-density detergent and high-density granular concentrated detergent, bulk density measurement method, and scent evaluation method are explained below, but the manufacturing method is a preferred example and is not particularly limited to this. isn't it. (1) Detergent manufacturing method From Composition 1 in Table 1, prepare a slurry with a moisture content of 50% by weight, excluding 2% by weight of zeolite and a small amount of additives such as enzymes and other components that are preferable to be dry mixed later. The powder obtained by spray-drying the powder was dry mixed with the components initially removed, thereby obtaining a low-density detergent of composition 1 having a bulk density of 0.30 g/cm ³ . On the other hand, from Composition 2 in Table 1, a slurry with a water content of 50% by weight was prepared with the composition excluding 10% by weight of zeolite and a small amount of additives such as enzymes, etc., which are preferable to be dry mixed later, and the slurry was sprayed. The powder obtained by drying is put into a high-speed mixer (agitating rolling granulator, manufactured by Fukae Kogyo Co., Ltd.), and 5% by weight of zeolite moistened with 1% by weight of water is added to crush and granulate. Grind and add 3% by weight of zeolite
By dry mixing the remaining 2% by weight of zeolite and a small amount of additives to the particles obtained by adding and crushing and granulating, a high-density granular concentrated detergent having a bulk density of 0.75 g/cm ³ and composition 2 was obtained. (Here, the water in the zeolite moistened with water added during crushing and granulation is
The zeolite acts as a granulation binder for the crushed detergent powder, and the zeolite acts as a water carrier for the granulation binder, and also as a granulation aid that suppresses the formation of coarse particles together with the subsequently added zeolite. Zeolite, which is dry mixed at the end, is mixed in both of the above two types of detergents for the purpose of improving the fluidity and anti-caking properties of the detergent particles. All of these zeolites are used in the form of fine powder. Additionally, a portion of the sodium carbonate in compositions 1 and 2 may be added during the final dry mixing, respectively). For each detergent obtained in this way,
A predetermined amount of the fragrance composition shown in Table 2 was spray mixed and left in a closed plastic bag at room temperature overnight, and then evaluated for aroma. (2) Measurement of detergent bulk density (apparent specific gravity) Measured by the method of JIS K-3362 (3) Evaluation of fragrance (i) Evaluation of fragrance of detergent powder Pour detergent into a wide-mouth glass bottle with a capacity of 100 cm ³ and add approximately 50 cm ³ of detergent.
Immediately after the lid was placed and the lid was opened, 10 trained panelists evaluated the strength of the scent using a paired comparison method with a standard detergent. As a reference detergent, composition A is added to 100 parts by weight of low density detergent of composition 1.
0.12 parts by weight of fragrance was used. The evaluation criteria are shown below. Evaluation points Evaluation criteria 2 Much stronger than the standard detergent 1 Slightly stronger than the standard detergent 0 Same as the standard detergent - 1 Slightly weaker than the standard detergent - 2 Much weaker than the standard detergent The evaluation results are based on the number of people who gave each rating and the number of people who gave each rating. It is expressed as the sum of products with the evaluation score. In other words, the larger the value, the stronger the scent. (ii) Evaluation of scent of laundry liquid: Add 40g of low-density detergent of composition 1 and 25g of high-density granular concentrated detergent of composition 2 to 30g of tap water at 20℃.
Immediately after dissolving in the washing machine, the strength of the scent of the washing liquid was evaluated in the same manner as in (i). (iii) Evaluation of scent lingering properties of washed clothes Add 1 kg of cotton underwear to the washing liquid used in (ii), wash for 10 minutes, dehydrate for 1 minute, and then wash at 20°C.
6 while running tap water at a flow rate of 15/min.
After rinsing for 3 minutes, dehydrating for 3 minutes, and air-drying indoors overnight, the strength of the scent lingering on cotton underwear was compared with that of cotton underwear treated in the same way with a standard detergent.
Evaluation was made in the same manner as (i).

[Table] As is clear from the above results, when the same fragrance composition as the reference detergent is added to high-density granular concentrated detergent at the same ratio (Comparative Example 1), the scent of the washing liquid and the residual scent of the clothes are reduced. However, when using almost the same amount of fragrance composition based on the weight of the detergent used (Comparative Example 3), the fragrance of the detergent powder becomes too strong.
In the middle (Comparative Example 2), the scent of the powder was a little strong, and the scent of the washing liquid and the residual scent of clothes were a little too weak. On the other hand, if the fragrance composition of the present invention was used, it was possible to give the fragrance characteristics almost the same as the standard detergent in all respects by selecting an appropriate fragrance ratio.

Claims (1)

[Scope of Claims] 1. A fragrance composition comprising 50 to 90% by weight of a fragrance component with a vapor pressure of 5 to 50 μHg, 40% by weight or less of a fragrance component with a vapor pressure of more than 50 μHg, and 20% by weight or less of a fragrance component with a vapor pressure of less than 5 μHg. In this case, a fragrance composition containing 20% by weight or more of one or more fragrance ingredients selected from the group consisting of (1) to (11) below in a fragrance ingredient with a vapor pressure of 5 to 50 μHg is blended. High-density granular concentrated detergent composition. (1) Dimethylbenzyl carbinyl acetate (2) Tricyclo[5.2.1.0 ^2.6 ]-dec-3-ene-
8-yl acetate (3) tricyclo[5.2.1.0 ^2.6 ]-dec-3-ene-
8-ylpropionate (4) 3-amyl-4-acetoxytetrahydropyran (5) 4-tert-butylcyclohexyl acetate (6) 2-tert-butylcyclohexyl acetate (7) p-tert-butyl-α-methyl Hydrocinnamic aldehyde (8) 4-(4-hydroxy-4-methylpentyl)
-3-Cyclohexene-1-carboxaldehyde (9) α-hexylcinnamic aldehyde (10) α-amyl cinnamic aldehyde (11) α,α-dimethyl-p-ethylhydrocinnamic aldehyde.