JPH01185400A - Method of imparting odor to powdery alkali detergent - Google Patents

Abstract

PURPOSE:To increase freedom of perfume odor regulation and effect odor regulation for powdery alkali detergents, by including a liq. perfume which is unstable to alkalis or has a high volatility by means of an inclusion compd. and adding the included perfume to a powdery detergent. CONSTITUTION:When odor is imparted to a powdery alkali detergent by means of a liq. perfume component (A) which is stable to alkalis and has a low volatility, such as an alcohol, an ester of a sec. or tert. alcohol, a ketone or an ether, and a perfume component (B) which is unstable to alkalis or has a high volatility, such as a monoterpene hydrocarbon or aldehyde, the component (A) is either directly sprayed to a powdery detergent stock or premixed with part of the detergent and then added as a pulverized master powder, and the component (B) is included by means of an inclusion compd. such as beta-cyclodextrin and then added as a perfume-including material, to thereby impart odor.

Description

[Detailed description of the invention] [Industrial application field] The present invention relates to a method for flavoring an alkaline powder detergent.

[Prior Art and Problems to be Solved by the Invention] Generally, perfumes are in liquid form (of course, there are also solid perfumes such as camphor) and are used for various purposes. One use is as an ingredient in powdered laundry detergents.
It is used for purposes such as masking raw materials and providing comfort to the user during use. Liquid perfumes can be easily added to liquid detergents, but no special efforts have been made for powder detergent systems. -For boat fishing,
A liquid fragrance is sprayed onto a powder system or mixed with some components of a cleaning agent in advance to form a powder and solidify it, which is then added as a so-called master powder.

Fragrances have functional groups such as hydroxyl groups, aldehyde groups, ester groups, ketone groups, nitro groups, amine groups, ether groups, cyano groups, or double bonds as numbering groups, and are generally used as heavy powder laundry detergents. Decomposes in alkaline systems such as agents,
Many are susceptible to denaturation or polymerization. Therefore, it is necessary to select an alkaline and stable fragrance material as the fragrance for the alkaline powder detergent, and the degree of freedom in creating fragrances has been limited. Furthermore, even if highly volatile fragrance materials such as monoterpene hydrocarbons are blended into cleaning agents, they quickly evaporate during manufacturing and product storage. There was a problem that the scent was different from that of the original.

West German Patent No. 3,020,269 discloses a technique for blending powdered detergent with a powdered fragrance obtained by including the fragrance in an inclusion compound such as cyclodextrin in order to maintain the fragrance.

This technology merely involves the inclusion of fragrance materials, such as those conventionally used in heavy powder laundry detergents.
Therefore, it has not yet been put to practical use, and it does not teach anything about the possibility of increasing the degree of freedom in perfume composition.

[Means to solve the problem]

As a result of intensive research to expand the degree of freedom in flavoring alkaline powder detergents, the inventors of the present invention discovered that the objective could be achieved by using clathrated fragrance materials that were conventionally considered unsuitable for alkaline detergents. The invention has been completed.

That is, in the present invention, a liquid fragrance material that is alkaline-based, stable, and has low volatility is sprayed onto powder detergent fabric, or added as a master powder that has been mixed with a part of the detergent ingredients in advance. Provided is a method for flavoring an alkaline powder detergent, characterized in that a stable or highly volatile liquid fragrance material is included in a compound having inclusion ability to form a fragrance clathrate, and then added to a powder detergent.

In the present invention, stable or unstable in alkaline systems refers to water-soluble or insoluble alkaline substances commonly used in alkaline detergents, such as carbonates, silicates, phosphates, zeolites, etc. It means stable or unstable.

Traditionally, commonly used alkaline, stable, and low volatility fragrance materials include alcohol, secondary or tertiary alcohol esters, ketones, and ethers, and the following fragrance materials are specifically exemplified. Ru.

(i) Alcohol synthetic sandals, penzylalconopephenyl ethyl alcohol, styralyl alcohol, dimethylbenzyl carbinol, etc. (ii) Ketontenchrome, acetophenone, benzophenone, α-
Damascone, methyl amyl ketone, etc. (iii) Ester hedeion, hexyl salicylate, isoamyl salicylate, flutate, methyl benzoate, etc. (iv) Ether diphenyl oxide, amyl phenyl ethyl ether Novesedrumba, Neroline Yarayara, Anethole, etc. (v) Others Aldehyde C-14 peach, coumarin, pentalide,
These fragrance materials, such as musk ambrette and methyl anisranilate, are conventionally added to powdered detergent fabrics by spraying or as a master powder mixed with some of the detergent ingredients.

The following are examples of alkaline fragrances that are unstable or highly volatile and have been considered unsuitable in alkaline fragrances.

(1) Monoterpene hydrocarbons and their derivatives (1) Monoterpene hydrocarbons limonene, α-pinene, β-pinene, tercupirun,
Myrcene, etc. (ii) Derivatives (alcohols) Citronellonobelinalol, geraniol, etc. (ketones) l-menthone, β-carvone, camphor, etc. (esters) Cinnamyl acetate, geranyl acetate, turbinyl acetate, etc. (aldehydes) Citral, citranella novel (Others) Citronellylnitrinopegeranylnitrile, eucalybutol, etc. (2) Aldehydes from 06 to CI5 excluding (1) 08
~C-aldehydes, lyral, anisaldehyde, benzaldehyde, α-n-7 milcinnamic aldehyde, α-n-hexyl cinnamic aldehyde, lilyal, heliotropine, cinnamic aldehyde, etc. (3) Excluding (1) <C5-C,5 formic acid or acetate ester benzyl formate, phenylethyl formate, anisyl acetate, benzyl acetate, phenylethyl acetate, cinnamyl acetate, p-tert-butylcyclohexyl acetate, isoamyl acetate, cis-3- One or more of the above perfumes, such as hexyl acetate, are blended into the alkaline powder detergent system as a perfume clathrate, which is clathrated with a compound having clathration ability.

The method of including the fragrance with an clathrate compound and turning it into powder can be the method used for boat fishing. Normally, it can be obtained by gradually adding a fragrance to a slurry or aqueous solution of the clathrate while stirring, and then filtering and drying the fragrance clathrate.

As the clathrate compound used in the present invention, β-cyclodextrin is best, but β-cyclodextrin derivatives such as methylated β-cyclodextrin, α-cyclodextrin, r-cyclodextrin, etc. can also be used.

The fragrance and the clathrate compound are used in a molar ratio of 1:0.8 to 1.2.

The fragrance inclusion powder obtained in this way can be used as it is depending on the fragrance material, but it is better to use it after granulation, which greatly improves the stability in alkaline systems. Even when clothes are washed three times, the odor emitted from the laundry can be masked.

Granulation of the powdered fragrance clathrate is carried out in a dry or wet manner using a binder. Here, dry granulation or wet granulation refers to whether or not water is used as a binder.For dry granulation without using water, the binder must have a melting point or softening point of 40℃~
An organic compound exhibiting a temperature of 160°C is used. Organic compounds having a melting point or softening point of 40°C to 160°C include:
Polyethylene glycol having a molecular weight of 1,500 to 20,000, polyethylene glycol alkyl ether having an alkyl group having 08 to C2□ polyethylene glycol alkyl phenol ether having an alkyl group having 012 to 22 carbon atoms, having an alkyl group having 012 to 37 carbon atoms Examples include fatty acids, block polymers of ethylene oxide and propylene oxide, and the like.

The powdered fragrance is granulated by an extrusion granulation method with the addition of a binder and, if necessary, a filler such as Glauber's salt and other additives.

In wet granulation using water, a binder such as carboxymethylcellulose is added if necessary, and granulation is carried out by extrusion granulation, transfer granulation, etc.

The particle size of the fragrance granules thus produced is determined by a sieve or the like to have an average particle diameter of 100 to 1000μ and 1000μ.
It is preferable to adjust so that the above amount is 5% by weight or less (hereinafter abbreviated as %), and the amount of 100μ or less is 5% or less.

In the present invention, fragrance ingredients that are unstable and easily volatilized are added as fragrance clathrates, and fragrance ingredients that are stable and difficult to volatilize in powder detergents are added as usual, which increases the degree of freedom in creating fragrances. be able to. Moreover, it is economically advantageous because the required amount of the clathrate compound can be reduced.

Mixed fragrances are usually added at around 0.1 to 0.5% in detergents.
will be combined. When preparing perfume, it is preferable that the ratio of the clathrated fragrance in the mixed fragrance is 80% or less to the total mixed fragrance.

The alkaline powder detergents to which the perfuming method of the present invention can be applied are not particularly limited; 10-60% surfactants such as sulfonates, higher fatty acid salts, and polyoxyethylene alkyl ethers; 30-80% alkaline detergents such as carbonates, silicates, phosphates, and zeolites; fillers such as Glauber's salt; , O~30% bleaching agents such as percarbonate and perborate, anti-redeposition agents such as polyethylene glycol and carboxymethyl cellulose, enzymes such as protease and cellulase, fluorescent brighteners, and other ingredients such as fragrances. Examples include those containing about 2 to 6%.

〔Effect of the invention〕

The fragrance-imparting method of the present invention increases the degree of freedom in blending fragrances,
It is now possible to give alkaline powder detergents an unprecedented scent.

〔Example〕

The present invention will be explained below with reference to Examples, but the present invention is not limited to these Examples.

Note that part 1% in the examples is 2% by weight.

The compositions of the fragrance and powder detergent used are shown below.

Fragrance composition> *Trans-2-hexanol 2% *Phenylethyl alcohol 40% *Phenylethyl-n-butyrate 5% (2) 2-Cyclohexylpropanal 3% (2) α-hexyl cinnamic aldehyde 5% (2) Anisaldehyde
5% [2] Cyclamenaldehyde
15% (3) Benzyl acetate
25%100% Rose fruity *Phenylethyl alcohol 55%*Phenylethyl ethyl alcohol) 20%*Vanillin
2% (2) Lilial
5% (2) Anisaldehyde 3% (3) Benzyl acetate 5% (3) Phenylethyl acetate 10% 100% Lemon Muguet tone * Phenylethyl alcohol 20% (1) Limonene 20% (1) Citral 5% (2) Lilial 10% (2)
α-hexyl cinnamic aldehyde 20% (2) Lyral 15% [3) Benzyl acetate 10% 100% <Powder detergent composition> A spray-dried detergent composition having the following composition was prepared.

Softanol 120 3.0% beef tallow fatty acid sodium soap 2.8% sodium carbonate
10.0% No. 2 sodium silicate
9.5% 4A type zeolite 2
3.5% Sodium Sulfate Balanced Polyethylene Glycol 6000 2.0% Carboxymethyl Cellulose 1.5% Tinopal CaS
<Fluorescent dye) 0.35% water
4.5% total
100% Example 1 100 parts of the above powdered detergent was sprayed with (A) 0.2 parts of the above blended fragrance (B) The fragrance ingredients marked with * in the above blended fragrance were sprayed, and other fragrance ingredients were added using the method below. (C) Spray the fragrance ingredients marked with * in the above-mentioned blended fragrance, and remove the other fragrance ingredients by the following method. A granulated fragrance inclusion body powder was obtained, and the mixture (fragrance content in the detergent was 0.2 parts) was evaluated for the stability of the fragrance and the persistence of the odor.

<Preparation of fragrance inclusion body powder and its granules> Celldex N (manufactured by Japan Food Processing Co., Ltd.) was poured into 200 companies of 60°C hot water.
18.0 g of β-cyclodextrin) was added,
- Completely dissolves the cyclodextrin. 2.5g of the following blended fragrance was added to this and stirred for 3 hours. After addition of the prepared fragrance, a water-insoluble precipitate was formed and an inclusion phenomenon was observed.

After filtration, 20 g of fragrance inclusion complex powder was obtained by freeze-drying. After mixing the inclusion body powders with the following composition, a granulated product was obtained using an extrusion granulator manufactured by Nipaudal Co., Ltd. (model IEXKs-1). This was classified using a 16.32 mesh sieve to obtain a granulated product.

Particle size distribution of granules; average particle size: 670 μm 000 μm or more 1.0% Less than 100 μm 4.0%
Place the sample in a sample bottle, seal it, and store at -5℃, 30℃, and 40℃.
The fragrance was stored for 20 days, and the stability of the fragrance was determined by sensory evaluation. There were 4 scent panelists (male 25 years old, male 36 years old, female 36 years old)
I went there as a female (female x 8 years old). The results are shown in Table 1.

0 No change ○~△ Slight change △ Obvious change Table 1 □□- <Evaluation of odor persistence> Detergents (A), (B), and (C) were stored at room temperature (20°C), and immediately after production, After 10 days, 20 days, and 30 days, the clothes were washed under the following washing conditions, and the stability of the originally designed fragrance was evaluated at a practical level. The evaluation was determined by sensory evaluation (the panelists were the same as above). The results are shown in Table 2.

Washing machine Toshiba Galaxy 2.2kg Water amount 3H Detergent amount 40g Clothing 1kg (Cotton shirt 600g, T/C dress shirt 400g
g (item worn for one day) Washing time: 7 minutes. Lemon Muguet-like perfume was used as the perfume (A), (B), and (C).

Rating: 0 The same smell as when blending is present during washing. ○～△　Slightly different smell compared to when perfumed drifts while washing △　　Obviously different from when blending perfume The smell lingers while washing Table 2

Claims (1)

[Scope of Claims] 1. When flavoring an alkaline powder detergent with a fragrance consisting of an alkaline, stable and low volatile liquid fragrance component and an alkaline, unstable or highly volatile liquid fragrance component, A liquid fragrance ingredient that is stable and has low volatility in an alkaline system can be sprayed onto the powder detergent fabric, or it can be mixed with a part of the detergent ingredients in advance and added as a powdered master powder. 1. A method for flavoring an alkaline powder detergent, characterized in that a liquid fragrance component having a high oxidation rate is included in a compound having inclusion ability to form a fragrance clathrate, and then added to a powder detergent. 2. The method for flavoring an alkaline powder detergent according to claim 1, wherein the fragrance clathrate is granulated. 3. The method for scenting an alkaline powder detergent according to claim 1 or 2, wherein the fragrance to be clathrated is 80% by weight or less based on the total fragrance. 4. The alkaline compound according to any one of claims 1 to 3, wherein the compound having inclusion ability is one or more selected from the group consisting of β-cyclodextrin, derivatives thereof, α-cyclodextrin, and γ-cyclodextrin. How to add fragrance to powdered detergent.