JP2002003339A - Multilayer type composition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a multilayer type composition that can form a cloudy emulsion layer, with the oil component is stably kept in emulsion form, and further to obtain a multilayer type composition that can be clearly separated into original multilayers in a short time, after the composition is stirred and allowed to stand. SOLUTION: The objective liquid mutilayer type composition that can include stably emulsified layer characteristically comprises a nonionic surfactant with HLB of 2-7, an oily component and water.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

[0001] The present invention relates to a liquid multilayer composition containing an emulsified layer. More specifically, by shaking at the time of use, the cloudy emulsified layer that had been separated is uniformly dispersed throughout and becomes a whole cloudy state, and after being used, the cloudy emulsified layer is separated again to form a multilayer. To form a multilayer composition.

[0002]

2. Description of the Related Art In many cases, a multilayer composition comprising two or more layers is composed of two layers, an oil layer and an aqueous layer or an aqueous layer and a powder layer. All of these are made into a uniform milky liquid and powder dispersion by shaking at the time of use, and after standing, the dispersed oil and powder gather at the upper or lower part and become multilayer again. It is.

[0003] Of these, in the case of a multilayer composition formed from an oil layer and a water layer, the appearance of both layers is almost transparent, and it is difficult to see at a glance that the composition is a multilayer type. There are problems such as being incorrect or the features of the product being difficult to understand from the appearance. This problem can be solved if at least one layer is an opaque emulsified layer. For this reason, a surfactant is blended to form an emulsified layer, but it is difficult to make the emulsified layer exist stably, and it is easily separated into water and oil. Moreover, even if it is left to stand after shaking at the time of use, it does not become a multilayer containing an emulsified layer.

[0004]

DISCLOSURE OF THE INVENTION The present invention has been made in view of the above circumstances, and has as its object to form an emulsified layer and an other layer which stably form an emulsified layer while maintaining an emulsified state of oil. The present invention further provides a multilayer composition comprising: shaking the composition, breaking the multilayer, and, when left standing, separating the original multilayer in a short time and cleanly. is there.

[0005]

Means for Solving the Problems The inventors of the present invention have conducted intensive studies to solve the above-mentioned problems, and as a result, by combining a nonionic surfactant having an HLB of 2 to 7 with an oily component, A multilayer composition having good stability of the emulsified layer and a beautiful appearance is obtained.When the composition is shaken and allowed to stand, a multilayer composition that separates into the original multilayer in a short time is obtained. As a result, the present invention has been completed.

That is, the present invention relates to a liquid multilayer composition comprising a multilayer including an emulsified layer, characterized by containing a nonionic surfactant having an HLB of 2 to 7, an oil component, and water. is there.

[0007] The present invention also provides the above liquid multilayer composition, wherein the nonionic surfactant having an HLB of 2 to 7 is a compound having no polyoxyethylene chain.

Further, the present invention is the above-mentioned liquid multilayer composition, wherein the nonionic surfactant having an HLB of 2 to 7 is a glycerin fatty acid ester or a polyglycerin fatty acid ester.

Further, the present invention is the above liquid multilayer composition, wherein the multilayer composition is a multilayer composition comprising an emulsified layer and an aqueous layer.

[0010] As an example of compounding a surfactant, there is a multilayer composition in which a small amount of a surfactant is compounded for the purpose of facilitating the use and the emulsion composition is temporarily emulsified during shaking. The oil which has been temporarily emulsified gradually coalesces with time after standing to form large oil droplets and collects on the upper portion to form a transparent oil layer, resulting in a transparent multilayer composition.

[0011]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, embodiments of the present invention will be described in detail.

The multilayer composition of the present invention is a whole liquid composition comprising an emulsified cloudy emulsified layer and other layers. In the present invention, examples of other layers include an aqueous layer and an oil layer, and an aqueous layer is preferable. When the composition of the present invention is shaken at the time of use, the cloudy emulsified layer that has been separated is uniformly dispersed throughout to become a whole cloudy state, and by standing after use, the cloudy emulsified layer is separated again. To the original multilayer composition. The emulsified layer may be either a water-in-oil type or an oil-in-water type. In order to produce the multilayer composition of the present invention, a production method based on general emulsification means is used. For example, in an aqueous phase in which a water-soluble component is dissolved, the present invention in which ethanol is dissolved in ethanol is specified. Is dissolved, and the oil phase is added to the aqueous phase to emulsify.

The nonionic surfactant used in the present invention has an HLB of 2 to 7. Preferably, 2-
Five. These nonionic surfactants can have various structures for both hydrophilic groups and hydrophobic groups (lipophilic groups), and depending on the structure, sorbitan fatty acid esters, glycerin fatty acid esters, polyglycerin fatty acid esters, and propylene glycol fatty acid esters. , POE derivatives and the like.

The following are specific examples. The number in parentheses indicates the value of HLB.

Sorbitan monoisostearate (5.
0), sorbitan monostearate (4.7), sorbitan monopalmitate (6.7), sorbitan monooleate (4.3), sorbitan tristearate (2.
Sorbitan fatty acid ester such as 1), glycerin monoisostearate (4.0), glyceryl monostearate (2.0), glycerin monopalmitate (4.
0), glycerin fatty acid esters such as glyceryl monooleate (3.2), diglycerin monoisostearate (5.5), diglycerin monostearate (5.
0), polyglycerin fatty acid esters such as diglycerin monooleate (5.5), diglycerin diisostearate (2.0), diglycerin distearate (2.0), diglycerin dioleate (7.0), Propylene glycol fatty acid esters such as propylene glycol monostearate (3.5), propylene glycol monooleate (2.0), propylene glycol monolaurate (4.0), polyoxyethylene (1 mol addition) stearate (2 .0) (hereinafter, polyoxyethylene is also referred to as POE, and the number of moles of polyoxyethylene added is simply represented by a numeral), POE (2) stearate (4.0), POE (4) stearate (6 .5),
POE (2) oleate (4.5), POE (2) cetyl alcohol (3.2), POE (2) oleyl alcohol (2.5), POE (3) castor oil (3.0), P
POE derivatives such as OE (5) hydrogenated castor oil (6.0) and POE (10) hydrogenated castor oil (6.5).

In the present invention, a compound having a structure having no POE chain as a hydrophilic group is preferable in that the time required for separation into two layers is further shortened. Particularly, glycerin fatty acid esters and polyglycerin fatty acid esters are preferable. In the present invention, the above nonionic surfactants can be used alone or in combination of two or more.

In the present invention, the content of the nonionic surfactant having an HLB of 2 to 7 is preferably in the range of 0.01 to 10% by mass, more preferably 0.05 to 2% by mass. Further, 0.1 to 1% by mass is most preferable. When the amount is less than 0.01% by mass, the emulsified state cannot be sufficiently stabilized. On the other hand, when the amount exceeds 10% by mass, the speed of the two-layer separation decreases. In addition, the transparency and the usability of the aqueous layer also deteriorate.

As the oily component used in the present invention, any oily component which is usually used in pharmaceuticals, quasi-drugs, cosmetics, toiletries, sundries and the like can be used. Liquid oils such as olive oil, avocado oil, evening primrose oil, jojoba oil, cocoa butter,
Solid oils such as coconut oil, mocro kernel oil, waxes such as beeswax, candelilla wax, carnauba wax, hydrocarbon oils such as squalane, liquid paraffin, vaseline, paraffin, microcrystalline wax, isocetyl isostearate, di-2-ethylhexanoic acid ethylene glycol,
Ester oils such as 2-ethylhexanecetyl, trimethylolpropane tri-2-ethylhexanoate, pentaerythritol tetra-2-ethylhexanoate, glyceride tri-2-heptylundecanoate, diisobutyl adipate and 2-hexyldecyl sebacate , Chain silicone oils such as dimethylpolysiloxane and methylphenylpolysiloxane, octamethylcyclotetrasiloxane,
Cyclic silicone oils such as decamethylcyclopentasiloxane, stearic acid, behenic acid, 12-hydroxystearic acid, isostearic acid, eicosapentaenoic acid,
Examples include higher fatty acids such as docosahexaenoic acid and higher alcohols such as cetyl alcohol, behenyl alcohol, butyl alcohol, cholesterol, phytosterol, and isostearyl alcohol. These oily components can be used alone or in combination of two or more.

In the present invention, the content of the oily component is generally from 1 to 70% by mass.

In the present invention, water is contained as an essential component. The water content is generally between 1 and 99% by weight.

The multilayer composition of the present invention can be widely applied to pharmaceuticals, quasi-drugs, cosmetics, toiletries, miscellaneous goods and the like.

In the multilayer composition according to the present invention, in addition to the above-mentioned essential components, if necessary, components generally incorporated in the above-mentioned products such as cosmetics as long as the effects of the present invention are not impaired. Can be blended. As those ingredients,
Lower alcohols such as ethanol and isopropyl alcohol; polyhydric alcohols such as glycerin, propylene glycol, dipropylene glycol, 1,3-butanediol, sorbitol and maltitol; talc, kaolin, titanium oxide, silicic anhydride, cellulose powder Water-soluble polymers such as polyvinylpyrrolidone, polyvinyl acetate, carboxymethylcellulose, and xanthan gum; anionic surfactants; amphoteric surfactants;
Fungicides; ultraviolet absorbers; chelating agents; antioxidants; coloring agents such as dyes and pigments;

[0023]

EXAMPLES The present invention will be specifically described below with reference to examples, but the present invention is not limited to these examples. The compounding amount is mass%. Prior to the examples, the evaluation method used in each example will be described.

[Emulsification stability test] A sample was kept at 45 ° C for one month.
After that, the turbidity of the emulsified layer, the state of separation of the oil component, and the like were observed and evaluated according to the following criteria. ：: no change in the turbidity of the emulsified layer, no separation of oil was observed. Δ: turbidity of the emulsified layer was slightly transparent, but no separation of oil was recognized. ×: turbidity of the emulsified layer was considerably transparent. But separation of oil is not observed XX: Separation of oil is observed

[Measurement of Two-layer Separation Speed] Glass sedimentation tube (capacity 100 ml, outer diameter 30 mm, height 250 mm, 1
100 ml sample)
Put into a constant temperature bath at 30 ° C. and leave until the temperature reaches 30 ° C. When the temperature reached 30 ° C., the sedimentation tube was inverted about 25 times for 1 minute to disperse the content sample well, and then allowed to stand again in a thermostat at 30 ° C. Twenty-four hours after that, the volume of the lower layer is measured in a state of separation into two layers. The evaluation of the two-layer separation speed differs depending on the lower volume when the equilibrium state is reached. For example, when the lower volume in the equilibrium state is 80 ml, it is sufficient if the value in 24 hours is half or more of 40 ml or more. It can be determined that the separation speed is high, and when the separation speed is about 0 to 10 ml, it is determined that the separation speed is low.

[Aqueous layer transparency test] Glass sedimentation tube (capacity 100 ml, outer diameter 30 mm, height 250 mm, 1
100 ml sample)
And left in a thermostat at 30 ° C. for 24 hours to separate into two layers. The sedimentation tube was placed in front of the black plate, and the transparency of the aqueous layer was observed with the naked eye, and judged based on the following criteria. ：: almost transparent △: slightly transparent but slightly cloudy ×: cloudy and almost transparent

[Usability test] About 1 ml of a sample was applied to the face of 10 female panels in their 20s and 30s, and a questionnaire on the feeling of use was taken, and evaluated according to the following criteria. ○: Two or less panelists answered “sticky” △: Three or more panelists answered “sticky” ×: Six or more panelists answered “sticky” Was

A multilayer composition having the composition shown in Tables 1 and 2 was prepared. That is, glycerin was added and dissolved in purified water. Next, glyceryl monoisostearate or a mixture of glyceryl monoisostearate EO adduct and a preservative dissolved in ethanol were mixed. next,
Liquid paraffin and pentaerythyl tetraoctanoate were added and emulsified by strong stirring. These compositions were subjected to a stability test, a two-layer separation speed measurement, a transparency test and a usability test of an aqueous layer (lower layer) after separation. It should be noted that the lower layer volume when reaching the equilibrium state in each experiment was prescribed so as to be substantially the same. In Table 1, POE5, POE1
The numbers of 5, 15, 30, and 60 of 5, POE30 and POE60 represent the number of moles of POE added.

[0029]

[Table 1] ―――――――――――――――――――――――――――――――――― Example Comparison Example ――― ――― ――――――――――― Component name 1 1 2 3 ――――――――――――――――――――――――――――――――― -Glyceryl monoisostearate 0.2---(HLB4) Glyceryl monoisostearate-0.2--(POE15) (HLB12) Glyceryl monoisostearate--0.2-(POE30) (HLB16) Glyceryl monoisostearate- --0.2 (POE60) (HLB19) Liquid paraffin 5.55 5.5 pentaerythyl tetraoctanoate 5.55 ethanol 5.55 5.5 glycerin 5.55 5 5 preservatives proper amount proper amount proper amount purified water residue residue-- ―――――――――― ――――――――――――――――――――――― Emulsion stability ○ × × ×× Bilayer separation speed (ml) 80 78 72 65 Transparency of aqueous layer ○ ○ △ △ Usability ○ ○ ○ ○ ――――――――――――――――――――――――――――――――――――

As is clear from Table 1, the multilayer composition of the present invention has good emulsion stability, a high two-layer separation speed, and is excellent in transparency and usability of the aqueous layer.

[0031]

[Table 2] ―――――――――――――――――――――――――――――――――― Examples ―――――――― ――――――――――――― Component name 2 3 4 5 6 ―――――――――――――――――――――――――――――― Glyceryl monoisostearate 0.01 0.2 2 10 15 (HLB4) squalane 55 55 55 pentaerythyl tetraoctanoate 55 55 55 ethanol 55 55 55 glycerin 55 55 55 preservative Appropriate amount Appropriate amount Appropriate amount Appropriate amount Purified water Residue Residue Residue Residue Residue ○ ○ ○ ○ ○ Two-layer separation speed (ml) 82 80 77 68 63 Transparency of aqueous layer ○ ○ ○ ○ × Usability ○ ○ ○ ○ × ―――――――――――――――― - -----------------

As apparent from Table 2, when the amount of the surfactant is 10% by mass, the bilayer separation speed is slightly lowered, and when the amount is 15% by mass, the transparency and the usability (stickiness) of the aqueous layer are deteriorated. Become like

Example 7 A multilayer cosmetic having the following composition was prepared. [Prescription] (1) Diglyceryl monostearate 3 (2) Glycerin 2 (3) Dipropylene glycol 2 (4) Decamethylcyclopentasiloxane 10 (5) Methylpolysiloxane 5 (6) Citric acid 0.1 (7) ) Sodium citrate 0.3 (8) Methylcellulose 0.1 (9) Sodium carboxymethylcellulose 0.1 (10) Ethanol 10 (11) Preservative proper amount (12) Flavor proper amount (13) Purified water residue [Production method] (13) (2), (3) and (6) to (9) are added and dissolved. Next, (10), (1) and (11)
A solution obtained by dissolving (12) is mixed. Next, (4) and (5)
And emulsify by adding strong stirring. A multi-layered cosmetic having good emulsion stability, a high two-layer separation speed, and good useability and transparency of the aqueous layer was obtained.

Hereinafter, in the same manner as in the seventh embodiment,
A multilayer cosmetic having the composition of Example 12 was prepared. In each case, a multi-layered cosmetic having good emulsion stability, a high two-layer separation speed, and good useability and transparency of the aqueous layer was obtained.

Example 8 [Prescription] (1) Sorbitan monooleate 0.5 (2) Glycerin 2 (3) Dipropylene glycol 2 (4) Decamethylcyclopentasiloxane 10 (5) Methylpolysiloxane 5 (6) Citric acid 0.1 (7) Sodium citrate 0.3 (8) Methylcellulose 0.1 (9) Sodium carboxymethylcellulose 0.1 (10) Ethanol 10 (11) Preservative appropriate amount (12) Dye appropriate amount (13) Purification Water residue

Example 9 [Prescription] (1) Tetraglycerin monostearate 0.1 (2) Glycerin 2 (3) Dipropylene glycol 2 (4) Decamethylcyclopentasiloxane 10 (5) Methylpolysiloxane 5 (6) ) Citric acid 0.1 (7) Sodium citrate 0.3 (8) Methylcellulose 0.1 (9) Sodium carboxymethylcellulose 0.1 (10) Ethanol 10 (11) Preservative proper amount (12) Flavor proper amount (13) Purified water residue

Example 10 [Prescription] (1) Propylene glycol monostearate 1 (2) POE (2) Stearate 0.1 (3) Glycerin 2 (4) Dipropylene glycol 2 (5) Decamethylcyclopentasiloxane 10 (6) methylpolysiloxane 5 (7) pentaerythritol tetra-2-ethylhexanoate 5 (8) citric acid 0.1 (9) sodium citrate 0.3 (10) methylcellulose 0.1 (11) carboxymethylcellulose Sodium 0.1 (12) Ethanol 10 (13) Preservative proper amount (14) Flavor proper amount (15) Purified water residue (16) Purified water residue

Example 11 [Prescription] Diglycerin diisostearate 2 Glycerin monooleate 1 (3) Glycerin 2 (4) Erythritol 0.5 (4) Dipropylene glycol 2 (5) Decamethylcyclopentasiloxane 10 (6) Methylpolysiloxane 5 (7) Citric acid 0.1 (8) Sodium citrate 0.3 (9) Methylcellulose 0.1 (10) Sodium carboxymethylcellulose 0.1 (11) Ethanol 10 (12) Preservative proper amount (13) ) Suitable amount of fragrance (14) Purified water residue

Example 12 [Prescription] (1) Diglycerin distearate 3 (2) Diglyceryl diisostearate 2 (3) Glycerin 10 (4) Dipropylene glycol 2 (5) Decamethylcyclopentasiloxane 10 (6) ) Methylpolysiloxane 5 (7) citric acid 0.1 (8) sodium citrate 0.3 (9) methylcellulose 0.1 (10) sodium carboxymethylcellulose 0.1 (11) ethanol 10 (12) preservative appropriate amount ( 13) Appropriate amount of fragrance (14) Purified water residue

[0040]

As described in detail above, according to the present invention,
Form a stable emulsified layer that is cloudy while the oil is kept in an emulsified state, and by shaking at the time of use, the separated emulsified layer is uniformly dispersed throughout and becomes a whole cloudy state, and is allowed to stand after use As a result, the cloudy emulsified layer is separated again to form the original multilayer, and at this time, the layer forming speed is high, and the liquid multilayer composition including the emulsified layer having a good appearance (the transparency of the aqueous layer is good). Things are obtained.

Claims (4)

[Claims] 1. A liquid multilayer composition comprising multiple layers including an emulsified layer, comprising a nonionic surfactant having an HLB of 2 to 7, an oil component, and water. 2. The liquid multilayer composition according to claim 1, wherein the nonionic surfactant having an HLB of 2 to 7 is a compound having no polyoxyethylene chain. 3. The liquid multilayer composition according to claim 1, wherein the nonionic surfactant having an HLB of 2 to 7 is a glycerin fatty acid ester or a polyglycerin fatty acid ester. 4. The liquid multilayer composition according to claim 1, wherein the multilayer composition is a multilayer composition comprising an emulsified layer and an aqueous layer.