JP2008163176A - Preparation of emulsion composition - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide an emulsion composition free from troubles of storage stability in formulating much perfume, capable of increasing lingering scent of the perfume on a treated fabric. <P>SOLUTION: The preparation of emulsion composition comprises (i) the process of heating a cationic surfactant (a) to a temperature not lower than the gel-liquid crystal transition temperature t1 (°C), (ii) the process of mixing the component (a) obtained in the process (i) with water heated at t1 to 100°C, (iii) the process of cooling the mixture obtained in the process (ii) to a temperature not higher than the t1 (°C), and (iv) the process of mixing a specific silicone emulsion (b) with the mixture obtained in the process (iii), wherein the preparation comprises the process adding a specific amount of the perfume (c) in either one of the processes (i)-(iv), or between each process, or after the process of (iv), and the invention relates to the emulsion composition prepared by the preparation and to the treated textile products containing the emulsion composition. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

  The present invention relates to a method for producing an emulsified composition, an emulsified composition obtained by the production method, and a fiber product treating agent containing the emulsified composition.

The technique which applies a silicone compound to textile products processing agents, such as a softening agent, is well-known, and can refer patent documents 1-4. Patent Document 5 can be referred to for the silicone emulsion.
JP 2004-131895 A JP 2004-131896 A JP 2004-263347 A JP-A-10-219567 JP 7-173294 A

  Generally, softeners and pastes are used to finish textile products. For example, softener compositions include cationic softener groups such as quaternary ammonium salts having a long-chain alkyl group and acid salts of tertiary amines. The agent is used and gives a high flexibility imparting effect to various fiber products. It is also known that silicone is blended in a softening agent to improve softening performance.

  On the other hand, generally a fragrance | flavor is mix | blended with the fiber treatment agent composition. Recently, in order to promote the deodorizing function of fragrances, and to increase the residual fragrance, studies have been made to increase the amount of fragrance added or to add a large amount of fragrance components with strong residual fragrance.

  However, generally a fragrance | flavor is an oil component, When it mix | blends abundantly, there exists a tendency for the storage stability of an emulsion composition to be impaired. Further, simply increasing the blending amount of the fragrance does not improve the residual scent strength of the treated cloth as expected, and further ingenuity is required.

  A textile treatment agent containing a cationic surfactant such as a conventional softener composition is mixed with a silicone compound at a temperature higher than the phase transition temperature of the cationic surfactant. A surfactant and a silicone compound coexist in the same emulsified particle and are present in the composition. Moreover, while the cationic surfactant and the silicone compound are uniformly emulsified, excellent storage stability can be obtained, but there is a problem that the effect of the silicone compound cannot be sufficiently obtained. As a method for solving this problem, it is preferable that the silicone particles and the cationic surfactant are present as separate particles in the composition, but in that case, there is a problem in storage stability.

  Accordingly, an object of the present invention is to provide an emulsified composition and a method for producing the same that can improve the remaining fragrance of the fragrance on the treated cloth without causing a problem in storage stability even if a large amount of the fragrance is blended. is there.

  The present inventor uses a silicone emulsion having a specific particle diameter obtained by emulsifying a silicone compound having a specific viscosity with a specific surfactant, and further, the fragrance and the silicone emulsion are converted into a cationic surfactant by a specific production method. It was found that an emulsified composition capable of improving the residual fragrance of the fragrance and solving the problem of storage stability can be obtained by mixing the fragrance with the fragrance, and the present invention has been completed.

  That is, the present invention comprises a cationic surfactant (a), a silicone emulsion (b) and a fragrance (c), which include the following steps (a), (b), (c) and (d). A method for producing an emulsion composition comprising 0.3 to 5% by mass at the same time as the following steps (a) to (e), or between each step, or after any step (d): A method for producing an emulsified composition comprising a step of adding a perfume (c) (amount relative to the final composition), an emulsified composition obtained by the production method, and a textile product treating agent containing the emulsified composition are provided. .

Step (a): The cationic surfactant (a) is heated to the gel-liquid crystal transition temperature t1 (° C.) or higher. Step (a): obtained in the step (a) with water at t1 to 100 ° C. Step (c) of mixing with the heated cationic surfactant (a): Step of cooling the mixture obtained in step (a) to a temperature below t1 (° C.) (D): A step of mixing the silicone emulsion (b) and the mixture obtained in the step (c)

<Silicone emulsion (b)>
5 to 70% by mass of a silicone compound (1) having a viscosity at 25 ° C. of 10,000 to 10,000,000 mm ² / s, 0.5 to 30% by mass of a nonionic surfactant (2), and A silicone emulsion containing water and having a volume average particle diameter of dispersed particles in the range of 300 to 800 nm.

  According to the production method of the present invention, it is possible to obtain an emulsified composition that has no problem in storage stability and can impart a higher residual fragrance property to the softener-treated cloth. The emulsified composition produced by the production method of the present invention sufficiently exhibits the effect of the silicone compound, and thus is suitable as a softener composition having excellent softness properties and excellent residual fragrance properties.

[Cationic surfactant (a)]
The cationic surfactant [hereinafter referred to as component (a)] used in the production method of the present invention preferably has a gel-liquid crystal transition temperature t1 of 0 to 90 ° C., more preferably 25 to 85, from the viewpoint of flexibility. ° C, more preferably 30 to 70 ° C. Examples of such cationic surfactants include tertiary amines having 1 to 3 hydrocarbon groups having 14 to 26 carbon atoms and the remainder being alkyl or hydroxyalkyl groups having 1 to 3 carbon atoms, or Its acid salt or its quaternized product is preferred. Specifically, it is suitable to be selected from the compounds represented by the following general formula (1). The gel-liquid crystal transition temperature is determined when a cationic surfactant solution is measured with a differential scanning calorimeter (DSC) according to the description in the literature: J. Phys. Chem. 1990, 94, 1550-1554. It is defined as the temperature of the maximum value (peak top) of the endothermic peak.

[Wherein, R ^1a is an alkyl group or alkenyl group having 14 to 26 carbon atoms which may be separated by an ester group, an amide group or an ether group, and R ^1b is an ester group, an amide group or an ether group. The alkyl group or alkenyl group having 14 to 26 carbon atoms, which may be divided, or the alkyl group or hydroxyalkyl group having 1 to 3 carbon atoms. R ^1c is a hydrogen atom, an alkyl group having 1 to 3 carbon atoms or a hydroxyalkyl group, and R ^1d is an alkyl group having 1 to 3 carbon atoms or a hydroxyalkyl group. X ⁻ represents an anionic group. ]
More specifically, the compound of the general formula (2) is preferable.

[Wherein, R ^2a is an alkyl group or alkenyl group having 14 to 24 carbon atoms, preferably 16 to 20 carbon atoms, and R ^2b is an alkyl group or hydroxyalkyl group having 1 to 3 carbon atoms, or R ^{2b 2f} — [B—R ^2g ] _d —. R ^2c is a hydrogen atom, an alkyl group having 1 to 3 carbon atoms or a hydroxyalkyl group, and R ^2d is an alkyl group having 1 to 3 carbon atoms or a hydroxyalkyl group. R ^2f is an alkyl group or alkenyl group having 14 to 24 carbon atoms. R ^2e and R ^2g are each independently an alkylene group having 1 to 6 carbon atoms. A and B are each independently a group selected from —COO—, —OCO—, —CONH—, and —NHCO—, and c and d are each independently a number of 0 or 1. X ⁻ represents an anionic group. ]

In the compound of the general formula (2), R ^2a is preferably an alkyl group or alkenyl group having 16 to 20 carbon atoms, and R ^2b is preferably a group represented by R ^2f — [B—R ^2g ] _d —. , R ^2f is preferably an alkyl group or alkenyl group having 16 to 20 carbon atoms. R ^2c and R ^2d are each independently preferably a methyl group or a hydroxyethyl group, and R ^2e and R ^2g are each independently preferably an ethylene group or a propylene group. A and B are each independently preferably —COO— or —CONH—, and c and d are preferably at least one of the numbers 1 and particularly preferably both are the numbers of 1. X ⁻ is preferably a halogen ion, an alkyl sulfate ion having 1 to 3 carbon atoms, or a fatty acid ion having 1 to 18 carbon atoms.

[Silicone emulsion (b)]
In the production method of the present invention, 5 to 70% by mass of the silicone compound (1) having a viscosity at 25 ° C. of 10,000 to 10,000,000 mm ² / s and 0.001 of the nonionic surfactant (2). A silicone emulsion (b) [hereinafter referred to as component (b)] containing 5 to 30% by mass and water and having a volume average particle diameter of dispersed particles in the range of 300 to 800 nm is used.

The silicone compound (1) having a viscosity at 25 ° C. of 10,000 to 10,000,000 mm ² / s (hereinafter referred to as “component (b1)”) has a dynamic (unified) viscosity at 25 ° C. of 100,000 to 6000, A highly polymerized silicone compound having a viscosity of 000 mm ² / s is preferred. Examples of the silicone compound that can be used include dimethylpolysiloxane, amino-modified silicone, and polyether-modified silicone, and dimethylpolysiloxane is most preferable from the viewpoint of softening effect. Above the lower limit of the viscosity range, sufficient flexibility can be exhibited, and below the upper limit of the viscosity range, the emulsion can be easily made fine. Specific examples of silicone compounds that can be used include highly polymerized dimethicone (25 ° C., kinematic viscosity 6,000,000 mm ² / s) manufactured by Shin-Etsu Silicone, and highly polymerized dimethicone SH200-1,000,000cs manufactured by Toray Dow Silicone. (Kinematic viscosity 1,000,000 mm ² / s).

The silicone emulsion (b) is in the form of an emulsion obtained by emulsifying the component (b1) with a nonionic surfactant (hereinafter referred to as the component (b2)). As the component (b2), a compound represented by the following general formula (3) is suitable.
R ^3a —O— (DO) _n —H (3)
[Wherein R ^3a is a hydrocarbon group having 10 to 22 carbon atoms, D is an ethylene group or a propylene group, and n is a number from 1 to 120 indicating the average number of added moles. ]

In general formula (3), R ^3a is preferably an alkyl group having 12 to 16 carbon atoms, D is preferably an ethylene group, n is preferably 1 to 120, more preferably 2 to 80, particularly preferably 3 to 3. 40. In the present invention, the lipophilic component (b2) and the hydrophilic component (b2) are preferably used in combination from the viewpoint of the stability of the emulsion. Specifically, the lipophilic component (b2) is generally used as a general component. In the formula (3), n is 1 to 9, preferably 2 to 8 [hereinafter referred to as the component (b21)], and the hydrophilic (b2) component is n in the general formula (3), preferably 10 to 50. Contains 10 to 30 compounds (hereinafter referred to as component (b22)) at a mass ratio of (b21) / (b22) = 0.05 to 2, preferably 0.1 to 0.5.

The component (b) according to the present invention preferably contains an anionic surfactant [hereinafter referred to as the component (b3)] for the purpose of further improving the stability of the emulsion. The compound (4) is preferred.
R ^4a -X (4)
[Wherein, R ^4a is an alkyl group having 10 to 16 carbon atoms or an alkylaryl group having 10 to 16 carbon atoms, and X is —SO ₃ M, — (OA) _m —OSO ₃ M . -(OA)-is an oxyethylene group or an oxypropylene group, and m is a number from 0 to 4 indicating the average number of moles added. M is an inorganic or organic cation. ]

  Specifically, an alkylbenzene sulfonate having 10 to 16 carbon atoms, an alkyl sulfate ester salt having 10 to 16 carbon atoms, preferably 10 to 14 carbon atoms, an average addition mole number of oxyethylene groups of 1 to 4, preferably 1.5 to 3. Polyoxyethylene alkyl ether sulfates having 10 to 16, preferably 10 to 14 carbon atoms in the alkyl group are suitable. The salt is preferably a sodium salt, potassium salt or alkanolamine salt.

  In the present invention, it is preferable to use the component (b2) and the component (b3) in combination, and the mass ratio of the component (b2) / (b3) is 10 to 300, more preferably 50 to 200, and particularly 70 to 150. It is preferable for the purpose of improving.

The component (b) according to the present invention is in the form of an emulsion obtained by emulsifying the above-mentioned component (b1), component (b2), and component (b3) in water, if desired. The volume average particle diameter is 300 to 800 nm, and this range is suitable from the viewpoint of easy mixing, storage stability, and softening effect.
The content of the component (b1) is 5 to 70% by mass in the component (b), more preferably 10 to 65% by mass, particularly preferably 30 to 60% by mass, and the content of the component (b2) is in the component (b). 0.5-30 mass%, Furthermore, 1-20 mass%, Especially 2-15 mass% is preferable. Further, the content of the component (b3) is preferably 0.001 to 5 mass%, more preferably 0.01 to 3 mass% in the component (b).

  Furthermore, the mass ratio of (b2) component / (b1) component is 0.02-0.3, more preferably 0.05-0.2, and the mass ratio of (b3) component / (b1) component is 0.00005- 0.005, more preferably 0.0005 to 0.002.

  Further, the water content in component (b) is preferably 10 to 65% by mass, more preferably 20 to 60% by mass, and particularly preferably 30 to 55% by mass.

  In order to prepare the component (b) containing dispersed particles having a volume average particle diameter in the above range, a method of emulsifying using a stirring device capable of applying a high-speed shearing force such as a homomixer or a high-pressure homogenizer is used. Can be mentioned. In addition, a so-called emulsion polymerization method in which a low-molecular cyclic polysiloxane is used as a starting material and is polymerized in the emulsified dispersion state using a strong acid or a strong alkali as a catalyst can also be employed. Preferably, the component (b1) and the component (b3) are added while applying high-speed shearing force to an aqueous solution containing part or all of the component (b2) and part or all of water with an apparatus such as a homomixer or a high-pressure homogenizer. The method of adding and mixing the remaining component (b2) and water is preferable, and the amount of the component (b2) used in the step of adding the component (b1) while applying high-speed shearing force is 20 to the total amount of the component (b2)). It is 100% by mass, preferably 20 to 70% by mass, particularly preferably 20 to 50% by mass. The volume average particle size can be measured using a submicron particle size measuring device (photon correlation method).

[Fragrance (c)]
Among compounds generally used as fragrances, fragrance components (c1) having a water / octanol partition coefficient (log P) of less than 3.0 and a vapor pressure at 20 ° C. exceeding 1.33 Pa are likely to evaporate. Normally, it does not remain in the clothes after washing or softening, but has a good fragrance property. On the other hand, the fragrance component (c2) having a water / octanol partition coefficient (log P) of 3.0 or more and a vapor pressure at 20 ° C. of 1.33 Pa or less tends to remain in clothes after washing and softening treatment, and has a residual fragrance property. Although it is a fragrance component having a fragrance, it has a property of weak smell.

  Although the fragrance | flavor (c) used by this invention is not restrict | limited in particular, By raising the residual fragrance | flavor property of the fragrance | flavor component (c1) and (c2) with sufficient balance, the fragrance standing immediately after fiber processing, and fragrance persistence Can be made compatible. The fragrance component (c1) preferably has a log P of 0 or more and less than 3, and the fragrance component (c2) preferably has a log P of 3 or more and 7 or less. The fragrance (c) of the present invention preferably contains 20 to 60% by mass of a fragrance component having a log P of 3 to 7 and a vapor pressure at 20 ° C. of 1.33 Pa or less. It is more preferable to contain 5 to 25% by mass of (c1).

  Specific examples of the fragrance component (c1) are shown in Tables 1 to 3. As the fragrance component (c1), phenylethyl alcohol and geraniol are particularly preferable.

  Specific examples of the fragrance component (c2) are shown in Tables 4-6. As the fragrance component (c2), lyial or hexylcinnamic aldehyde is particularly preferable.

[Method for producing emulsified composition]
The method for producing an emulsified composition of the present invention includes the step (a), the step (b), the step (c) and the step (e), and further, simultaneously with the steps (a) to (e) or each step. It includes a step of mixing 0.3 to 5% by mass (amount relative to the final composition) of the fragrance composition (c) in the middle of or after any step (d).

  In the step (a), the temperature for heating the component (a) is t1 ° C. or higher, preferably t1 to 90 ° C, more preferably t1 to 80 ° C, and particularly preferably t1 to 75 ° C.

  Moreover, in order to assist melting of the component (a), it is preferable to use a water-soluble solvent in combination with the component (a) in the step (a). Specific examples include ethanol, propanol, isopropanol, ethylene glycol, propylene glycol, and glycerin, with ethanol and isopropanol being particularly preferred. The content of the water-soluble solvent is preferably 2 to 40% by mass, more preferably 3 to 30% by mass, and particularly preferably 5 to 25% by mass with respect to the component (a).

  In the step (a), water heated to t1 to 100 ° C., preferably t1 to 90 ° C., more preferably t1 to 75 ° C., and the heated (a) component obtained in the step (a) are mixed. The mass ratio of component (a) / water is preferably 0.05 to 0.4, more preferably 0.07 to 0.3, and particularly preferably 0.1 to 0.25. By mixing with water having a temperature of t1 ° C. or higher, the component (a) does not precipitate and the dispersibility is improved.

  In the present invention, in step (a), a nonionic surfactant (hereinafter referred to as component (d)) is used for the purpose of assisting mixing of component (a) and obtaining a stable emulsion of component (a). Is preferred. As the component (d), a compound represented by the following general formula (5) is suitable.

^R5a- E-[( ^R5bO ) _e- ^R5c ] _g (5)
[Wherein, R ^5a is an alkyl group or alkenyl group having 8 to 18 carbon atoms, preferably 10 to 16 carbon atoms, and R ^5b is an alkylene group having 2 or 3 carbon atoms, preferably an ethylene group. R ^5c is an alkyl group having 1 to 3 carbon atoms or a hydrogen atom. e represents a number of 2 to 100, preferably 5 to 80, more preferably 10 to 70. E is —O—, —COO—, —CON— or —N—, and when E is —O— or —COO—, g is 1, and when E is —CON— or —N—. g is 1 or 2. ]

Specific examples of the compound of the general formula (5) include the following compounds.
R ^5a —O— (C ₂ H ₄ O) _h —H
[Wherein R ^5a has the above-mentioned meaning. h is a number of 8 to 100, preferably 10 to 70. ]
_{^{R 5a -O - [(C 2}} H 4 O) i / (C 3 H 6 O) j] -H
[Wherein R ^5a has the above-mentioned meaning. i and j are each independently a number of 2 to 40, preferably 5 to 40, and (C ₂ H ₄ O) and (C ₃ H ₆ O) may be random or block adducts. ]

[Wherein R ^5a has the above-mentioned meaning. k and l are each independently a number from 0 to 40, and k + 1 is a number from 5 to 70, preferably from 5 to 40. R ^5d and R ^5e are each independently a hydrogen atom or an alkyl group having 1 to 3 carbon atoms. ]

  In the step (a), the component (d) has a mass ratio of (d) component / (a) component of 0.01 to 0.6, more preferably 0.05 to 0.5, particularly 0.1 to 0.4. It is preferable to be used.

  In the step (a), the component (a) heated to t1 (° C.) or higher, the heated water, and optionally the component (d) are mixed with stirring. The stirrer is not particularly limited. In the present invention, it is preferable to use a milder from the viewpoint of stirring efficiency and stability of the mixture.

  In the present invention, it is preferable to adjust the pH after mixing the above-mentioned components in the step (a), and the pH is obtained when a small amount of the mixture obtained in the step (a) is obtained and cooled to 20 ° C. Is preferably 1 to 6, more preferably 1.5 to 5, and particularly preferably 1.7 to 4. Examples of pH adjusters include citric acid, acetic acid, malic acid, succinic acid, benzoic acid, benzenesulfonic acid, p-toluenesulfonic acid and other organic acids, hydrochloric acid, sulfuric acid, phosphoric acid and other inorganic acids, and water. Alkaline agents such as sodium oxide, potassium hydroxide, sodium carbonate, potassium carbonate, alkanolamine can be used.

Step (c) is a step of cooling the mixture of step (i) to a temperature below t1 (° C.), and the cooling temperature is preferably 0 ° C. or higher, more preferably 5 ° C. or higher, particularly preferably 10 ° C. or higher. It is preferably (t1-5) ° C. or lower, more preferably (t1-15) ° C. or lower.
Cooling is not particularly limited, but for example, a paddle type agitator, a propeller type agitator, a homomixer, a milder, a Claremix, a fillmix, an ultramixer, a line mixer, a Becomix, a lexamix, a static mixer Cooling with stirring, preferably using a propeller stirrer.

  In the present invention, the mixture obtained after cooling (hereinafter sometimes referred to as “cooled product”) preferably has an emulsion form in which the particles of component (a) are emulsified. Is preferably 10 to 300 nm, more preferably 20 to 200 nm, and particularly preferably 30 to 150 nm.

Step (d) in the present invention is a step of mixing the above-described component (b) and the cooling product obtained in step (c). Although not particularly limited, for example, a paddle type agitator, a propeller type agitator, a homomixer, a milder, a clear mix, a fill mix, an ultra mixer, a line mixer, a Becomix, a lexamix, and a static mixer are used with stirring. , Preferably using a static mixer under low shear.
The mixing ratio of the component (b) and the cooling material is such that [the mass of the silicone compound in the component (b)] / [the mass of the component (a) in the cooling material] = 0.01- 0.5 is preferable, and 0.02 to 0.3 is more preferable.

  In the emulsion composition obtained by such a method, the component (a) and the component (b1) are present as independent particles. The volume average particle diameter of the emulsified particles of component (a) is preferably 10 to 300 nm, more preferably 20 to 250 nm, particularly preferably 30 to 200 nm, and the volume average particle diameter of component (b1) is 300 to 800 nm, more preferably 350 to 700 nm. preferable. Even if the component (b1) is mixed in the step (d), the particle diameter does not change.

The above particle diameter is obtained from pulsed magnetic field gradient NMR measurement according to the method of literature: J. Colloid Interface Sci. 239, 535-542 (2001) under the temperature condition of 25 ° C. using the emulsified composition as it is as a measurement sample. be able to.

  In the method of the present invention, the fragrance (c) may be added in any of the steps (a) to (d) or between the steps (a) to (d). The fragrance (c) may be added at a plurality of locations after completion of the step (d), but the fragrance (c) may be added in a temperature range of t1 to 100 ° C. Preferably, it is added at the stage of step (a), or more preferably added between step (a) and step (c), and it is particularly preferred to add at step (a).

  The addition amount of the fragrance | flavor (c) is 0.3-5 mass% as an quantity with respect to a final composition, and 0.4-3 mass% is preferable.

[Emulsified composition and fiber product treating agent]
The emulsified composition produced by the method of the present invention is preferably applied to a textile product treating agent, particularly a softener composition added to rinsing water at the rinsing stage in the washing process. That is, the production method of the present invention can be applied to a method for producing a textile product treating agent, particularly a softener composition. When applied to a softener composition, the content of the component (a) is preferably 5 to 35% by mass, more preferably 10 to 30% by mass, and particularly preferably 15 to 25% by mass in the final composition. Content is 0.01-5 mass% in final composition, Furthermore, 0.05-3 mass%, Especially 0.2-2 mass% is preferable, The total content of (b2) component and (d) component is 0.5 to 10% by mass in the final composition, more preferably 0.7 to 7% by mass, particularly preferably 1 to 5% by mass, and the content of the component (c) is 0.3 to 5% by mass in the final composition, Furthermore, 0.4-3 mass% is preferable. The blending ratios of the components (a) to (d) and water in the production process are adjusted so as to have such a content. Moreover, when applying to a softening agent composition, an inorganic salt can be contained as (e) component other than said (a)-(d) component. As the inorganic salt, sodium chloride, calcium chloride, and magnesium chloride are preferable from the viewpoint of storage stability. However, although surfactants such as fatty acid salts include sodium salts and potassium salts, inorganic salts derived from these may also be included in the composition of the present invention. The content of the component (e) is 0.1 to 5% by mass, preferably 0.1 to 3% by mass, and particularly preferably 0.1 to 2% by mass in the softener composition. Moreover, it is preferable that (e) component melt | dissolves uniformly in the step of the said process (I).

  When the present invention is applied to a softener composition, a saturated or unsaturated fatty acid having 8 to 22 carbon atoms or a saturated or unsaturated fatty acid having 8 to 22 carbon atoms is used as component (f) for the purpose of improving storage stability. An ester compound of polyhydric alcohol can be blended. From the viewpoint of storage stability and softening effect, the compounds that can be blended include fatty acids selected from palmitic acid, stearic acid, oleic acid, linoleic acid, triglycerides, diglycerides, monoglycerides, mono-, di- or triesters of pentaerythritol, sorbitan esters Mention may be made of the ester compounds selected.

  The content of the component (f) is 0.1 to 5% by mass, preferably 0.1 to 3% by mass, and particularly preferably 0.1 to 2% by mass in the softener composition. Further, the component (f) is preferably added at the stage of the step (a) and dissolved uniformly.

  When applying the present invention to a softener composition, it can contain appropriately used dyes, antioxidants, viscosity modifiers, anti-gelling agents, hydrotropes, sequestering agents, etc. These are preferably dissolved uniformly at the stage of step (a).

Examples 1-15 and Comparative Examples 1-18
A fiber product treating agent having the composition shown in Tables 8 to 10 was prepared according to the following preparation method using the following blending components. The storage stability and residual fragrance property of the obtained textile product treating agent were evaluated by the following methods. The results are shown in Tables 8-10.

<(A) component>
As the component (a), (a-1) to (a-3) represented by the following formulas were used. (A-1) to (a-3) were produced by a known method or a method described in JP-A-11-229273.

<(B) component>
(B-1): Highly polymerized dimethicone emulsion Polyoxyethylene lauryl ether (b21) having a kinematic viscosity at 25 ° C. of 6,000,000 mm ² / s, 60% by mass of silicone oil (component b1), and an average EO addition mole number of 5 mol Component) 2% by mass, average EO addition mole number 23 mol of polyoxyethylene lauryl ether (b22 component) 5% by mass, sodium lauryl sulfate (b3 component) 0.1% by mass, water remainder, volume average particle diameter of dispersed particles 500nm
(B-2): Highly polymerized dimethicone emulsion Polyoxyethylene lauryl ether (b21) having a kinematic viscosity at 25 ° C. of 1,000,000 mm ² / s, 60% by mass of silicone oil (component b1), and an average EO addition mole number of 5 mol Component) 1.5% by mass, average EO addition mole number 23 mol of polyoxyethylene lauryl ether (b22 component) 4.5% by mass, sodium lauryl sulfate (b3 component) 0.1% by mass, water remainder, dispersed particles Volume average particle diameter 500nm

<(B ′) Component (Comparative Product of Component (b))>
(B′-1): Highly polymerized dimethicone emulsion Polyoxyethylene lauryl ether having a kinematic viscosity at 25 ° C. of 1,000,000 mm ² / s, 60% by mass (b1 component), and an average EO addition mole number of 5 mol ( b21 component) 2% by mass, average EO addition mole number 23 mol of polyoxyethylene lauryl ether (b22 component) 4.5% by mass, sodium lauryl sulfate (b3 component) 0.1% by mass, remaining water, volume of dispersed particles Average particle size 10μm
(B′-2): Dimethicone emulsion 60% by mass of a silicone oil having a kinematic viscosity of 5,000 mm ² / s at 25 ° C., 1.5% by mass of polyoxyethylene lauryl ether (b21 component) having an average EO addition mole number of 5 mol Polyoxyethylene lauryl ether (b22 component) having an average EO addition mole number of 23 mol, 5.5% by mass, sodium lauryl sulfate (b3 component) 0.1% by mass, remainder of water, volume average particle diameter of dispersed particles 500 nm
<(C) component>
(C-1): Perfume having the composition shown in Table 7 (c-2): Perfume having the composition shown in Table 7

<Other ingredients>
(D-1): An average of 20 moles of ethylene oxide added to a saturated primary alcohol having 12 carbon atoms (e-1): Calcium chloride

<Method for preparing textile product treating agent>
(1) Preparation method 1
In a 300 mL beaker, 95% of the amount of ion-exchanged water necessary for the finished mass of the fiber product treating agent to reach 200 g was added, and the temperature was raised to 70 ° C. in a water bath. While stirring with a turbine-type stirring blade having three stirring blades each having a length of 2 cm (300 r / min), required amounts of the components (d) and (e) were dissolved. Next, a required amount of the component (a) was added after heating to t1 (° C.) + 10 ° C. or more [steps (a) and (b)]. After stirring for 5 minutes, the pH was adjusted to the target pH with 35% aqueous hydrochloric acid and 48% aqueous sodium hydroxide, and 70 ° C. ion-exchanged water was added in an amount necessary for the final mass [step (b) ]]. Thereafter, the component (b) was added to the mixture. Thereafter, the mixture was stirred for 10 minutes, the beaker was transferred to a water bath containing 5 ° C. water, and the mixture was cooled to 20 ° C. while stirring to obtain a textile product treating agent. In addition, (c) component was added in the compounding liquid at the process shown in Tables 8-10. Moreover, pH shown to Tables 8-10 described pH after cooling (20 degreeC). The pH was adjusted with a 0.1N hydrochloric acid aqueous solution or a 0.1N sodium hydroxide aqueous solution. In the textile product treating agents in Tables 8 to 10, the component (a) is almost entirely present in the textile product treating agent in the form of hydrochloride.

(2) Preparation method 2
The steps (A), (I), and (I ′) were performed in the same manner as in Preparation Method 1. Thereafter, the mixture was stirred for 10 minutes, the beaker was transferred to a water bath containing 5 ° C. water, and the mixture was cooled to 20 ° C. while stirring [step (c)]. Thereafter, component (b) was added to the mixture [step (D)] to obtain a textile product treating agent. In addition, (c) component was added in the compounding liquid at the process shown in Tables 8-10. Moreover, pH shown to Tables 8-10 described pH after cooling (20 degreeC). The pH was adjusted with a 0.1N hydrochloric acid aqueous solution or a 0.1N sodium hydroxide aqueous solution. In the textile product treating agents in Tables 8 to 10, the component (a) is almost entirely present in the textile product treating agent in the form of hydrochloride.

<Evaluation method of storage stability>
The textile product treating agent was stored in a constant temperature room at 40 ° C. for 20 days, and the storage stability was determined according to the following criteria.
・ Storage stability evaluation criteria 3 points: No separation / precipitation is observed 2 points: Separation / precipitation is slightly observed 1 point: Separation / precipitation is observed 0 point: Separation / precipitation is remarkably observed If the stability evaluation score is 2 points or less, the solution state is not uniform, and therefore, it is not preferable because the softening effect and the remaining scent on the treated cloth cannot be uniformly imparted to the treated cloth.

<Evaluation method of residual fragrance>
(1) Preparation of evaluation towel 2 kg of commercially available cotton towel (100% cotton) was put into a fully automatic washing machine (National NA-F70E) and washed with a commercially available weakly alkaline detergent (attack manufactured by Kao Corporation). When rinsing, each fiber product treatment agent was used for treatment (standard course, detergent concentration 0.0667 mass%, textile product treatment agent amount 10 ml, tap water 40 L, water temperature 20 ° C.). Thereafter, the towel was naturally dried under conditions of 25 ° C. and 40% RH.

(2) Residual odor evaluation The residual fragrance of the treated towel was determined by 10 panelists (10 women in their 30s) according to the following criteria, and the average score was determined.
Evaluation criteria for residual fragrance 5: very fragrant 3: fragrant 1: not very fragrant 0: not fragrant In the residual fragrance evaluation point, 2.5 or more points are in good condition, and 3 or more points are very good. is there.

Claims (5)

Production of an emulsion composition comprising a cationic surfactant (a), a silicone emulsion (b) and a fragrance (c), comprising the following steps (a), (b), (c) and (d) It is a method and is 0.3-5 mass% (the quantity with respect to a final composition) at any one or more places after the following process (A)-(D) or between each process or after a process (D). The manufacturing method of the emulsion composition including the process of adding the fragrance | flavor (c) of).
Step (a): The cationic surfactant (a) is heated to the gel-liquid crystal transition temperature t1 (° C.) or higher. Step (a): obtained in the step (a) with water at t1 to 100 ° C. Step (c) of mixing with the heated cationic surfactant (a): Step of cooling the mixture obtained in step (a) to a temperature below t1 (° C.) (D): Step of mixing silicone emulsion (b) and mixture obtained in step (c) <Silicone emulsion (b)>
5 to 70% by mass of a silicone compound (1) having a viscosity at 25 ° C. of 10,000 to 10,000,000 mm ² / s, 0.5 to 30% by mass of a nonionic surfactant (2), and A silicone emulsion containing water and having a volume average particle diameter of dispersed particles in the range of 300 to 800 nm.   The manufacturing method of the emulsion composition of Claim 1 which adds a fragrance | flavor (c) in the temperature range of t1-100 degreeC.   The fragrance | flavor (c) contains 20-60 mass% of fragrance | flavor components whose water-octanol partition coefficient (logP) is 3-7, and whose vapor pressure in 20 degreeC is 1.33 Pa or less. Or the manufacturing method of the emulsion composition of 2.   The emulsion composition obtained by the manufacturing method in any one of Claims 1-3.   A textile product treating agent comprising the emulsified composition according to claim 4.