JP7680289B2 - Two-component solidifying composition - Google Patents

Description

The present invention relates to a two-component solidifying composition that is used primarily in peel-off pack cosmetics. More specifically, the present invention relates to a two-component solidifying composition that utilizes the solidifying reaction that occurs when xyloglucan and a polyhydric alcohol are mixed.

A gel-like peel-off type pack cosmetic is known in which a first agent containing xyloglucan and a second agent containing polyhydric alcohols are mixed at the time of use, the mixture is applied to the skin, and peeled off after solidification. The mechanism by which gelation occurs is as follows: xyloglucan molecules aggregate due to the dehydrating action of sugars and alcohols, and the sugars and alcohols further form a high-order network through hydrogen bonds with the xyloglucan molecules, resulting in gelation (in this specification, the term is used synonymously with solidification unless otherwise specified).
The two-component solidification composition utilizing such a mechanism of gelation has the following problems.
(i) It was necessary to shorten the solidification time as much as possible (shortening solidification time).
(ii) Regarding the mixing time, in order to mix the first and second parts uniformly, it was necessary to mix them for a long time. Some users would apply the product in an uneven state before it was completely mixed, in which case the desired performance could not be achieved. Therefore, it was necessary to shorten the mixing time (shortening the mixing time).
(iii) Concerning ease of use, if the ingredients cannot be mixed uniformly, the mixture will be patchy and difficult to apply. Therefore, there has been a demand for a product that is easy to mix uniformly and easy to spread (ease of spreading).
In addition, there was a problem that the mixture would drip while waiting for it to solidify after mixing, and therefore it was necessary to prevent this dripping (prevention of dripping).
Furthermore, if the strength of the pack is low, there is a problem that it may break when it is peeled off after being applied to the entire face. Therefore, it was necessary for the pack to be easy to peel off even after solidification, and to maintain a strength sufficient to prevent tearing (ease of peeling and pack strength).
(vi) Regarding stability, a certain level of storage stability was required for both the first and second formulations (storage stability).

Meanwhile, techniques for gel packs utilizing a solidification reaction between xyloglucan and alcohol are known, for example, as disclosed in the following Patent Documents 1 and 2.
Patent Document 1 discloses a solidifying composition containing a polyhydric alcohol having 3 or less OH groups, which is a two-part solidifying composition consisting of (A) a first part containing tamarind gum and (B) a second part containing polyglycerin in which 4 to 40 glycerin units are polymerized, and which solidifies by mixing and reacting when used.
This composition uses polyglycerin to accelerate the solidification speed, and also contains a thickener (hydrophobic cellulose) to improve the mixability during mixing, dripping during application, and peel-off properties. However, the gelation time is long, at over 5 minutes, and no consideration is given to the mixing time or stability.

Patent Document 2 describes a gelled aerosol product which includes a first container filled with a first agent, a second container filled with a second agent, and a propellant, and has an ejection mechanism for ejecting the first agent and the second agent, in which the first agent contains one of the following (A) and (B) and tamarind gum, and the second agent contains the other of the following (A) and (B), as well as glycerin and a diol having 2 to 6 carbon atoms:
(A) at least one selected from the group consisting of locust bean gum, glucomannan, tara gum, and guar gum; and (B) xanthan gum. A gelling aerosol product is disclosed, which is characterized by being gelled by mixing the ejected first agent and the second agent.
This product, by blending (A) and (B), is able to suppress syneresis and has a quick gelation time of less than 5 minutes; however, the mixing time for gelation is long at 1 minute, and no consideration is given to stability.
As described above, there are two-component solidifying compositions that attempt to solve some of the problems necessary for peel-off type pack cosmetics, but none of them have shortened the gelling time and mixing time, and furthermore, there is no technology yet that solves all of the problems, including those related to usability (ease of spreading, prevention of dripping, ease of peeling, and pack strength) and storage stability.

Patent No. 6459189 Patent No. 6490322

The present invention aims to solve the problems of the conventional technology described above, and aims to provide a two-component solidifying composition that has a short solidifying time and mixing time, as well as excellent usability (ease of spreading, prevention of dripping, ease of removal (peel-off properties), and appropriate pack (coating film) strength) and storage stability.

The present invention has been made to solve the above-mentioned problems, and as a result of extensive investigation into various compositions, it has been found that by combining xyloglucan, a polyhydric alcohol, and a specific thickener (an alkyl acrylate copolymer and/or an alkyl acrylate-methacrylate copolymer), it is possible to realize a two-component solidifying composition which has short solidifying and mixing times and which is excellent in terms of usability (ease of spreading, prevention of dripping, ease of removal (peel-off properties), and appropriate pack strength) and storage stability, and has thus completed the present invention.
That is, the present invention has the following configuration.
＜1＞
A two-part solidification composition that gels by mixing (1) a first part and (2) a second part shown below,
(1) A first agent containing water and xyloglucan; (2) A second agent containing a polyhydric alcohol. The two-component solidifying composition is characterized in that at least one of an alkyl acrylate copolymer and an acrylic acid/alkyl methacrylate copolymer is contained in at least one of the first agent and the second agent.
＜2＞
The two-component solidifying composition according to <1> above, wherein the polyhydric alcohol comprises at least one selected from the group consisting of glycerin, butylene glycol, dipropylene glycol, isopentyl diol, propane diol and diglycerin.
＜3＞
The two-agent solidifying composition according to <1> or <2> above, which is a peel-off pack in which the first agent and the second agent are mixed, applied to the skin to gel, and then peeled off.

By combining xyloglucan, polyhydric alcohol and a specific thickener (alkyl acrylate copolymer and/or alkyl acrylate-methacrylate copolymer), it has become possible to shorten the solidification time and mixing time. Furthermore, it has become possible to provide a two-component solidifying cosmetic that has excellent usability (easy spreading, prevention of dripping, ease of removal (peel-off properties), and appropriate pack strength) and excellent stability.

(Two-part solidification composition)
By mixing the first and second agents, xyloglucan reacts with polyhydric alcohol to form a crosslinked structure and gel. By adding a specific thickener to the first and/or second agents, the solidification time and mixing time can be shortened, and the solidified composition has excellent usability such as peel-off property and excellent stability.
The two-component solidifying composition of the present invention is a two-component solidifying composition that gels by mixing (1) a first component and (2) a second component shown below,
(1) a first agent containing water and xyloglucan;
(2) a second agent containing a polyhydric alcohol;
The two-part solidifying composition is characterized in that a specific thickening agent is contained in at least one of the first part and the second part.
As the specific thickener, an alkyl acrylate copolymer and an alkyl acrylate-methacrylate copolymer are used.
Therefore, in the two-part solidifying composition of the present invention, the composition obtained after mixing the first and second parts contains at least one of an alkyl acrylate copolymer and an acrylic acid/alkyl methacrylate copolymer.
The combination of the specific thickener in the first agent and/or the second agent will be described later.

(Xyloglucan)
The xyloglucan contained in the first agent of the present invention has a basic structure in which xylose is bonded as a side chain to a main chain in which glucose is bonded via β-1,4 bonds. It may also have a basic structure in which galactose is bonded as a side chain.
In this specification, the term "xyloglucan" includes high molecular weight (natural) xyloglucan. The term "xyloglucan" is mainly (95% or more) made of high molecular weight (natural) xyloglucan.

High molecular weight xyloglucan is a xyloglucan derived from a natural product, and can be obtained by extraction from, for example, the cell walls of higher plants such as pea, soybean, poplar, rice, bamboo shoots, and tamarind seeds (Tamarindus indica).
The molecular weight of high molecular weight xyloglucan is about 50,000 to 1,000,000.
The polymeric xyloglucan (tamarind seed xyloglucan) may be a commercially available product (e.g., Glyloid, Glyate, molecular weight 470,000, manufactured by DSP Gokyo Food & Chemical Co., Ltd.). Alternatively, a commercially available polymeric xyloglucan may be dissolved in water, and the aqueous solution may be mixed with ethanol or the like to separate and precipitate the xyloglucan, which may then be further purified. The polymeric xyloglucan may be partially decomposed to make it easier to use, and may contain a low molecular weight product. However, it is preferable to adjust the polymeric xyloglucan to 95% by mass or more of the total amount of the solid composition. Xyloglucan is known as tamarind gum (a gum obtained from tamarind seeds). The xyloglucan of the present invention preferably has a molecular weight of 300,000 to 600,000, more preferably 350,000 to 550,000.

The solidification composition of the present invention contains high molecular weight xyloglucan as xyloglucan, and is mainly composed of high molecular weight xyloglucan. The solidification composition may contain low molecular weight xyloglucan, which is obtained by depolymerizing high molecular weight xyloglucan, within a range that does not impair the effects of the present invention. It may also be a mixture of xyloglucans derived from multiple types of plants.

The content of xyloglucan in the solidifying composition can be adjusted appropriately so that when the first and second agents are mixed together, they form an aqueous gel while maintaining good viscosity, and are easy to peel off when used as a peel-off cosmetic.

The xyloglucan content is preferably 0.1 to 15% by mass, more preferably 0.3 to 10% by mass, even more preferably 0.75 to 5% by mass, and particularly preferably 2 to 4% by mass, based on the total amount of the solidified composition (after mixing the first and second agents). When the xyloglucan content is 0.1% by mass or more, the gel strength is high and the composition can be easily peeled off from the skin. When the xyloglucan content is 15% by mass or less, the viscosity of the aqueous solution does not become too high when the xyloglucan is dissolved in water, and the first and second agents can be easily mixed at the time of use. By appropriately adjusting the xyloglucan content, the gel strength and the viscosity of the aqueous solution can be controlled, and the desired liquid properties can be obtained.

In the present invention, by mixing the first and second agents at the time of use, the xyloglucan reacts with the polyhydric alcohol to form a cross-linked structure and gel. Considering the size of the container used in actual use, it is preferable that the first and second agents are discharged and mixed at a mass ratio of about 1:5 to 5:1. In other words, assuming that the first and second agents are mixed in the range of 1:5 to 5:1, the amount of xyloglucan to be contained in the first agent can be calculated from the preferred range of xyloglucan content after mixing described above.

The first agent contains water in addition to xyloglucan. Since the first agent of the present invention contains xyloglucan and water in advance, the viscosity of xyloglucan can be well maintained. Water is contained in the first agent, but may also be contained in the second agent.
The water used in the present invention may be any water that can be used in cosmetics, external medicines, quasi-drugs, etc. Purified water, distilled water, membrane-filtered water, and ion-exchanged water are preferred.
The water may be used alone or in combination of two or more of the above.
In addition to water and xyloglucan, the first agent preferably contains a polyhydric alcohol as an optional component. When the first agent contains a polyhydric alcohol, the xyloglucan is dispersed in water without forming lumps, and is dispersed quickly, which is preferable because it is easy to manufacture. In addition, when the first agent contains a polyhydric alcohol having antibacterial properties, the antiseptic effect of the first agent is increased, which is preferable. The polyhydric alcohol contained in the first agent is preferably such that the solidification is not completed by the first agent alone, and is preferably in an amount. Specifically, butylene glycol and pentylene glycol are preferable, and in the case of butylene glycol, 3 to 8% by mass of the total amount of the first agent is preferable, and in the case of pentylene glycol, 0.3 to 3% by mass of the total amount of the first agent is preferable.

(Polyhydric alcohol; contained in the second agent)
The second agent of the present invention essentially contains a polyhydric alcohol. The xyloglucan of the first agent reacts with the polyhydric alcohol of the second agent to form a crosslinked structure and gel. The polyhydric alcohol also serves to smooth the physical properties of the composition and to stabilize the product.
In the present invention, by combining xyloglucan, a polyhydric alcohol, and a specific thickener (alkyl acrylate copolymer and/or alkyl acrylate-methacrylate copolymer) described below, the solidification time and mixing time are shortened, and a two-part solidifying composition that is excellent in all aspects of usability (ease of spreading, prevention of dripping, ease of removal (peel-off property), and appropriate pack strength) and storage stability is realized. By combining two or more types of polyhydric alcohol, it becomes easier to adjust the desired mixing time and solidification time, and further, it becomes easier to adjust the usability to a preferred one depending on the purpose. Therefore, it is more preferable to combine two or more types of polyhydric alcohol in order to make fine adjustments.
The polyhydric alcohol used in the solidifying composition of the present invention refers to a dihydric or higher alcohol that can be used in general external preparations. Examples include, but are not limited to, polyglycerols such as glycerin, diglycerin, triglycerin, and tetraglycerin, butylene glycols such as ethylene glycol, 1,3-butylene glycol, and 1,4-butylene glycol, propylene glycol, isopentyl diol, dipropylene glycol, polyethylene glycol, propane diols such as 1,3-propane diol, 1,2-pentane diol, sorbitol, polyglycerol derivatives, reducing sugars such as glucose, fructose, glyceraldehyde, lactose, arabinose, and maltose, and sugar alcohols such as erythritol, maltitol, sorbitol, and xylitol. Of these, it is preferable to contain one or more of glycerin, butylene glycol, dipropylene glycol, isopentyl diol, propane diol, and diglycerin. In the present invention, the second agent may contain two or more, three or more, or four or more types of polyhydric alcohols.
In addition, as a combination of two or more polyhydric alcohols, it is preferable that at least one is selected from butylene glycol, dipropylene glycol, and isopentyl diol, and it is even more preferable that two or more are selected from butylene glycol, dipropylene glycol, and isopentyl diol.

The content of the polyhydric alcohol in the solidifying composition of the present invention may be appropriately adjusted so that when the first and second agents are mixed, a crosslinked structure is formed between the xyloglucan and the polyhydric alcohol, the composition has a suitable viscosity, and the solidifying time and mixing time are as desired. The content of the polyhydric alcohol (when two or more types are contained, the total amount) is preferably 15 to 55% by mass, more preferably 18 to 50% by mass, and even more preferably 20 to 40% by mass, based on the total amount of the solidifying composition (after mixing the first and second agents). A polyhydric alcohol content of 15% by mass or more is preferable because the pack solidifies, making it easier to mix and apply to the skin during use. A polyhydric alcohol content of 55% by mass or less is preferable because it allows for uniform mixing, prevents dripping, and improves usability.

When a polyhydric alcohol is optionally contained in the first agent for the purpose of preserving the composition or facilitating production, it is advisable to incorporate the polyhydric alcohol in the first agent within the range of the preferred content of polyhydric alcohol described above and to the extent that it does not solidify.

(alkyl acrylate copolymer, acrylic acid/alkyl methacrylate copolymer)
The solidified composition of the present invention is characterized by containing an alkyl acrylate copolymer and/or an alkyl acrylate-methacrylate copolymer as a specific thickener to impart appropriate viscosity and other properties. By blending these specific thickeners, the solidification time and mixing time can be further shortened. In addition, after xyloglucan and polyhydric alcohol are mixed, they do not react immediately, and crosslinks between xyloglucan and polyhydric alcohol are gradually formed, so that the solidified composition of the present invention can be mixed uniformly when used. In this way, by adopting the configuration of the present invention, the composition can be mixed uniformly without being unevenly formed due to a sudden solidification of a part during mixing, making it easier to spread. Furthermore, dripping can be prevented by increasing the viscosity. In addition, the strength of the solidified composition is increased, and the ease of peeling off the coating film when used as a pack is improved. Furthermore, even if a specific thickener (alkyl acrylate copolymer and/or alkyl acrylate-methacrylate copolymer) is contained in the first agent (containing xyloglucan) or the second agent (containing polyhydric alcohol), it does not adversely affect the storage stability of each agent before mixing, and stability can be guaranteed even after storage for one month under harsh conditions at 50°C.

The acrylic acid/alkyl methacrylate copolymer is a compound called "ACRYLATES/C10-30 ALKYL ACRYLATE CROSSPOLYMER", and is also called (alkyl) modified carboxyvinyl polymer, (alkyl) modified carbopol, (alkyl) modified carbomer, (acrylates/alkyl acrylate (C10-30)) crosspolymer, etc.
The alkyl acrylate copolymer is a compound called an "acrylates copolymer."
Examples of commercially available acrylic acid/alkyl methacrylate copolymers include those sold under the trade names "Carbopol ETD2020 polymer", "PEMULEN TR-1", and "PEMULEN TR-2" (all manufactured by Lubrizol Advanced Materials). Examples of commercially available alkyl acrylate copolymers include those sold under the trade name "Aculyn™ 33A" (manufactured by Rohm and Haas).

The solidified composition of the present invention after mixing the first and second agents needs to contain at least one of these thickeners, and the combination of the thickeners in the first and second agents before solidification is not important. Therefore, examples of combinations in which a specific thickener is mixed in the first and second agents include the following.
The following is an embodiment in which only either the alkyl acrylate copolymer or the acrylic acid/alkyl methacrylate copolymer is contained in the present composition.
(a) either the first or second agent contains an alkyl acrylate copolymer; (b) either the first or second agent contains an acrylic acid/alkyl methacrylate copolymer; (c) both the first and second agents contain an alkyl acrylate copolymer; and (d) both the first and second agents contain an acrylic acid/alkyl methacrylate copolymer.

The following are some embodiments in which both an alkyl acrylate copolymer and an alkyl acrylate-methacrylate copolymer are included in the present composition.
(A) The first agent contains both an alkyl acrylate copolymer and an acrylic acid/alkyl methacrylate copolymer, and the second agent does not contain these.
(B) The second agent contains both an alkyl acrylate copolymer and an acrylic acid/alkyl methacrylate copolymer, but the first agent does not contain either of them.
(C) The first agent contains an alkyl acrylate copolymer, and the second agent contains an acrylic acid/alkyl methacrylate copolymer.
(D) The first agent contains an acrylic acid/alkyl methacrylate copolymer, and the second agent contains an alkyl acrylate copolymer.
(E) Both the first and second agents contain both an alkyl acrylate copolymer and an acrylate-alkyl methacrylate copolymer.

The content of the specific thickener in the solidifying composition of the present invention may be appropriately adjusted so that when the first and second agents are mixed, a crosslinked structure is well formed between the xyloglucan and the polyhydric alcohol, resulting in an aqueous gel with appropriate viscosity and properties. The content of the specific thickener (total amount when two types are used) is preferably 0.001 to 5% by mass, more preferably 0.005 to 1% by mass, even more preferably 0.005 to 0.5% by mass, and even more preferably 0.01 to 0.5% by mass, based on the total amount of the solidifying composition (after mixing the first and second agents). When the content of the specific thickener is in the range of 0.001 to 5% by mass, appropriate mixing and solidifying times can be achieved, and the viscosity of the solidifying composition can be easily adjusted. If the amount is less than 0.001% by mass or exceeds 5% by mass, it may be difficult to obtain any of the following improvements: mixing time, solidification time, ease of mixing during use, ease of application to the skin, or strength when peeling off.

(pH)
The solidifying composition of the present invention is preferably adjusted to a pH of about 5 to 8 when used. When the pH is about 5 or more when used, there is no irritation due to acid, and no pain is caused when applied. Furthermore, when the pH is about 8 or less when used, there is no protein denaturing action due to alkali. The pH can be adjusted by water-soluble acids such as carbonates that can be used in the solidifying composition of the present invention, as well as salts of organic or inorganic acids and bases such as sodium hydroxide, potassium hydroxide, triethanolamine, and arginine.

(Other additives)
Other additives may be used in the first and second agents to the extent that the effect of the invention is not impaired. For example, known surfactants, fragrances, etc. may be added. The configuration of the present invention, i.e., "(1) a first agent containing water and xyloglucan, (2) a second agent containing a polyhydric alcohol, and at least one of an alkyl acrylate copolymer and an alkyl acrylate-methacrylate copolymer is contained in at least one of the first and second agents," provides a two-agent solidification composition that does not require other thickeners or water-soluble polymers and has a short solidification time and mixing time, and further provides a two-agent solidification composition that is excellent in usability (ease of spreading, prevention of dripping, ease of peeling (peel-off property), and appropriate strength of the pack (coating film)) and storage stability. However, for the purpose of finely adjusting the feel when applied to the skin, thickeners other than xyloglucan, alkyl acrylate copolymer, and alkyl acrylate-methacrylate copolymer can also be added. In addition, any active ingredient, such as a cosmetic ingredient when used as a pack agent, can also be added.
Other additives may be added to either the first or second agent.

(form of existence)
In the solidifying composition of the present invention, before use, water and xyloglucan are encapsulated in the first agent, and the polyhydric alcohol is encapsulated in the second agent, and the first agent and the second agent are in a separated form. As described above, the specific thickener is contained in either one or both of them.
For example, the composition may be in the form of a kit including a first container containing the first agent and a second container containing the second agent. The first and second containers can be opened and the first and second agents can be mixed to form a gel.
The form of the gel forming kit is not particularly limited as long as it is a container in which the first agent and the second agent can be filled and stored separately and can be taken out as appropriate, and examples thereof include a bottle container, a pump container, a cup container, a jar container, a tube container, a pouch container, a pack container, and a bag.

The solidified composition of the present invention contains xyloglucan, polyhydric alcohol, and a specific thickener, and thus can shorten the solidification time and mixing time, and has storage stability. Since xyloglucan and water are mixed in advance, the viscosity of xyloglucan can be well maintained. The solidified composition of the present invention contains a specific thickener, and therefore xyloglucan and polyhydric alcohol do not react immediately after mixing, and can well form crosslinks. In addition, the solidified composition is easy to spread on the skin during application, does not drip easily, and after use, the solidified composition (pack) can be easily and cleanly removed from the skin without breaking and remaining on the skin.
Because of these properties, the solidified composition of the present invention can be preferably provided as a peel-off type pack cosmetic having excellent usability.

The first agent is a liquid or gel containing xyloglucan and water. The second agent essentially contains a polyhydric alcohol. The second agent may further contain water. Either the first agent or the second agent, or both, contain a specific thickener (alkyl acrylate copolymer and/or acrylic acid-alkyl methacrylate copolymer). The second agent is a liquid or gel (including a cream). The water and xyloglucan content in the first agent, the polyhydric alcohol content in the second agent, and the specific thickener content in the first agent and/or the second agent are as described above.

The mixing ratio of the first agent and the second agent may be appropriately adjusted so as to achieve the above-mentioned preferred embodiment.
The mixing ratio of the first agent and the second agent is not particularly limited since it depends on the concentration of each raw material in the first agent and the second agent, but the mixing ratio of the first agent and the second agent (mass of the first agent: mass of the second agent) is preferably 1:5 to 5:1, and more preferably 1:4 to 4:1. This is because the first agent and the second agent can be easily mixed within the above range.
The present invention will be explained in detail by the following tests (Examples 1 to 4 and Comparative Example).
In this test, the mixing ratio of the first agent and the second agent was 2:1, 3:1, and 4:1 by mass. In each test, xyloglucan was blended into the first agent, and polyhydric alcohol was blended into the second agent as an essential component. Polyhydric alcohol was also blended into the first agent from the viewpoint of ease of preparation and preservation. Tests were conducted in Test Example 1 to examine the specific thickener (a test in which it was blended into the first agent, and a test in which it was blended into the second agent).
The components used in the test were as follows:
- Xyloglucan: Glyloid 6C (molecular weight 470,000) manufactured by DSP Gokyo Food & Chemical Co., Ltd.

Test Example 1: Study on types of thickeners Various thickeners to be blended in the first or second agent were evaluated.
In addition, the specific thickener, alkyl acrylate copolymer or alkyl acrylate/methacrylate copolymer, is a component that is generally neutralized before use, and therefore sodium hydroxide is used as a neutralizing agent in the examples of this test.
[Test Example 1-1] When a thickener was blended in the first agent (1) Preparation of test samples The first agents (a-2 to a-15) and the second agent (b-19) shown in Table 1 were prepared. 8.0 g of the prepared first agent and 2.0 g of the second agent were weighed into a 20 mL cup and mixed with a spatula (1st agent: 2nd agent = 4:1), and the mixture was applied to a glass plate (soda-lime glass) with a finger, and each item was evaluated. The units in the table are "mass %".

(2) Evaluation Items and Criteria The following eight items were evaluated ((viii) Evaluation of stability was performed only for the first agent containing the specific thickener). The evaluation was performed by a specialist sensory evaluator.
(i) Mixing time The first and second agents were mixed with a spatula, and the time until a uniform gel was formed was measured. That is, the start of mixing was defined as 0 seconds, and mixing was stopped when a composition that was uniform and had enough viscosity to not run off the spatula (gel-like) was visually observed, and the time required was defined as the mixing time.
<Judgment criteria>
○: Within 30 seconds △: More than 30 seconds but less than 1 minute ×: 1 minute or more
(ii) Solidification time After mixing the first and second agents until they were uniform, the mixture was spread on a glass plate with a finger, left to stand, and the time until it was solidified uniformly and peeled off was measured. That is, the time when the mixture was completely spread was set to 0 seconds, and the state of the coating film was continuously observed visually until the entire coating film was solidified and peeled off was judged to be possible, and the observation was stopped, and the time required was recorded as the solidification time.
<Judgment criteria>
○: 3 minutes or less △: More than 3 minutes but less than 5 minutes ×: 5 minutes or more
(iii) Ease of spreading The homogenized mixture was spread on a glass plate with a finger. The ease of spreading was evaluated based on the properties (smoothness) and viscosity of the mixture at that time. The evaluation was performed while the mixture was being spread on the glass plate with a finger.
<Judgment criteria>
〇: Easy to spread (smooth and even application, appropriate viscosity and good spreadability)
△: A little difficult to spread, but it can be applied evenly, so it is within the acceptable range (high viscosity and poor spreadability, but spreadable)
×: Difficult to spread and cannot be spread (uneven properties, high viscosity, poor spreadability)
(iv) Dripping: After the mixture was applied to a glass plate with a finger, the glass plate was placed at a right angle to a desk, and the degree of dripping of the mixture was visually observed and evaluated according to the following criteria.
<Judgment criteria>
〇: No dripping △: Slight dripping ×: Dripping
(v) Properties of Pack When the solidified composition (pack) was peeled off from the glass plate, the state of the pack (film) was evaluated according to the following criteria.
<Judgment criteria>
〇: Smooth and uniform ×: Uneven
(vi) Ease of Peeling of Pack When the solidified composition (pack) was peeled off from the glass plate, the ease of peeling was evaluated according to the following criteria.
<Judgment criteria>
◯: Peelable evenly △: Slight tearing during peeling (within acceptable range as peelable)
×: Breaks when peeled off. (vii) Strength of Pack The hardness of the solidified composition (pack) when pressed with a finger was evaluated according to the following criteria.
<Judgment criteria>
〇: Hard and does not crumble when pressed with fingers △: Crumbs slightly when pressed with fingers ×: Crumbs easily when pressed with fingers
(viii) Stability A test sample was placed in a glass container having a diameter of 3 cm, and stored in a high-temperature room at 50° C. for one month. After that, the stability was evaluated by visual observation according to the following criteria.
<Judgment criteria>
〇: Stable ×: Unstable (separates)

(3) Evaluation results The results are shown in Table 2. The composition in Table 2 was calculated by measuring the first agent (8.0 g) and the second agent (2.0 g) into a 20 mL cup, mixing them with a spatula, and converting the solidified composition (10.0 g) after mixing into a 100 mass% composition.
Examples 1 and 2 achieved excellent results in all evaluation items. On the other hand, Comparative Examples 19 to 30 did not satisfy any or all of the items. Among these, Comparative Example 26, which used the hydrophobized cellulose used in the prior art (Patent Document 1), had a relatively short mixing time and was easy to spread, but after solidification, it was non-uniform, with unsolidified parts remaining and it was brittle.
From the above results, it was found that when an alkyl acrylate copolymer or an acrylic acid/alkyl methacrylate copolymer was used as the specific thickener, a satisfactory evaluation was obtained in all items.

[Test Example 1-2] When a thickener is added to the second agent
(1) Preparation of test samples The first agent (a-16) and the second agent (b-20 to 33) shown in Table 3 were prepared. 8.0 g of the prepared first agent and 2.0 g of the second agent were weighed into a 20 mL cup and mixed with a spatula (first agent:second agent=4:1), and the mixture was applied to a glass plate (soda-lime glass) with a finger, and each item was evaluated.

(2) Evaluation Items and Criteria Eight items were evaluated in the same manner as in Test Example 1-1, in which a thickener was blended in the first agent (the evaluation of stability in (viii) was performed only for the second agent containing the specific thickener). The evaluation was performed by a specialist sensory evaluator. b-20 is a composition that does not contain a thickener.

(3) Evaluation results The results are shown in Table 4. The compositions in Table 4 were prepared by weighing out the first agent (8.0 g) and the second agent (2.0 g) into a 20 mL cup, mixing them with a spatula, and converting the solidified composition (10.0 g) after mixing into a 100 mass% composition.
Examples 3 and 4 achieved excellent results in all evaluation items. Comparative Examples 33 to 42 were not able to be prepared because b-24 to b-33 of the second agent separated immediately after preparation and each thickener could not be blended. It should be noted that b-21 to b-23 were able to blend the thickener into the second agent. However, the stability of b-23 could not be guaranteed.
Comparative Examples 31 and 32 had a long solidification time of 10 minutes, and also had many other evaluation items rated as x.
From the above results, it was found that when an alkyl acrylate copolymer or an acrylic acid/alkyl methacrylate copolymer was used as the specific thickener, a satisfactory evaluation was obtained in all items.

Next, the details and results of the tests conducted in the process of arriving at the present invention are shown. The following test examples are compositions (comparative examples) that do not contain specific thickeners (alkyl acrylate copolymer and alkyl acrylate/methacrylate copolymer).

[Test Example 2] Evaluation of polyhydric alcohol in the second agent (1)
Regarding the polyhydric alcohol to be blended in the second agent, an evaluation was carried out when only one type was blended without any combination.
(1) Preparation of test samples The first agent (a-1) and the second agent (b-1 to b-11) shown in Table 5 were prepared. 6.0 g of the prepared first agent and 2.0 g of the second agent were weighed into a 20 mL cup, mixed with a spatula (first agent:second agent=3:1), and applied to a glass plate (soda-lime glass) with a finger, and each item was evaluated. The unit is "mass %".

(2) Evaluation Items and Criteria The following five items were evaluated by a professional sensory evaluator.
(i) Mixing time The first and second agents were mixed with a spatula, and the time until a uniform gel was formed was measured. That is, the start of mixing was defined as 0 seconds, and mixing was stopped when a composition that was uniform and had enough viscosity to not run off the spatula (gel-like) was visually observed, and the time required was defined as the mixing time.
<Judgment criteria>
○: Within 30 seconds △: More than 30 seconds but less than 1 minute ×: 1 minute or more
(ii) Solidification time After mixing the first and second agents until they were uniform, the mixture was spread on a glass plate with a finger, left to stand, and the time until it was solidified uniformly and peeled off was measured. That is, the time when the mixture was completely spread was set to 0 seconds, and the state of the coating film was continuously observed visually until the entire coating film was solidified and peeled off was judged to be possible, and the observation was stopped, and the time required was recorded as the solidification time.
<Judgment criteria>
○: 3 minutes or less △: More than 3 minutes but less than 5 minutes ×: 5 minutes or more
(iii) Ease of spreading The homogenized mixture was spread on a glass plate with a finger. The ease of spreading was evaluated based on the properties (smoothness) and viscosity of the mixture at that time. The evaluation was performed while the mixture was being spread on the glass plate with a finger.
<Judgment criteria>
〇: Easy to spread (smooth and even application, appropriate viscosity and good spreadability)
△: A little difficult to spread, but it can be applied evenly, so it is within the acceptable range (high viscosity and poor spreadability, but spreadable)
×: Difficult to spread and cannot be spread (uneven properties, high viscosity, poor spreadability)
(iv) Dripping: After the mixture was applied to a glass plate with a finger, the glass plate was placed at a right angle to a desk, and the degree of dripping of the mixture was visually observed and evaluated according to the following criteria.
<Judgment criteria>
〇: No dripping △: Slight dripping ×: Dripping
(v) Overall evaluation of the pack's usability (overall evaluation of the pack's properties, ease of removal, and strength)
The state of the solidified composition when it was peeled off from the glass plate and the hardness when pressed with a finger were evaluated according to the following criteria.
<Judgment criteria>
◯: Smooth, hard and evenly peelable, and does not break when pressed with a finger. ×: Brittle and uneven, and breaks when peeled off. In the table, "-" indicates that no evaluation was performed.

(3) Evaluation Results The results are shown in Table 6.
Comparative Examples 1 to 11 showed that the usability, such as the mixing time and solidification time, differed depending on the sample. Specifically, the dihydric polyhydric alcohols of Comparative Examples 1 to 4 had a fast solidification time but a long mixing time. The compositions containing trihydric and tetrahydric polyhydric alcohols of Comparative Examples 5 to 6 and sugar alcohols of Comparative Examples 7 and 8 had a slow solidification time but a short mixing time. Comparative Examples 9 to 11 were unable to be evaluated because they aggregated and did not form a pack.

[Test Example 3] Evaluation of two types of polyhydric alcohols (2)
Regarding the polyhydric alcohols to be blended in the second agent, evaluation was performed when two or more types were combined.
(1) Preparation of test samples First agent (a-1) and second agent (b-12 to b-18) shown in Table 7 were prepared. 6.0 g of the first agent and 3.0 g of the second agent were mixed (first agent:second agent=2:1), applied to a glass plate, and evaluated for each item.

(2) Evaluation Items and Criteria As in Test Example 2, evaluation was performed on five items.

(3) Evaluation Results The results are shown in Table 8.
From the test results of Comparative Examples 12 and 13, it was found that one type of polyhydric alcohol did not satisfy all the requirements.
On the other hand, although Comparative Examples 14 to 18 do not satisfy all items, it was found that by combining two types of polyhydric alcohol, items such as mixing time, solidification time, and ease of spreading were improved compared to when a single type was used.
From the above results, it was found that it is more preferable to use a combination of two or more polyhydric alcohols.

(Summary of Test Examples 1 to 3)
It was found that a two-component solidified cosmetic preparation having excellent usability, such as solidification time, mixing time, and peel-off property, and excellent stability, can be realized by combining xyloglucan, a polyhydric alcohol, and an alkyl acrylate copolymer and/or an alkyl acrylate/methacrylate copolymer. It was also found that a combination of two or more types of polyhydric alcohol is more preferable.

According to the present invention, by combining xyloglucan, polyhydric alcohol and a specific thickener (alkyl acrylate copolymer and/or alkyl acrylate-methacrylate copolymer), it is possible to shorten the solidification time and mixing time, and further provide a two-component solidified cosmetic that has excellent usability (ease of spreading, prevention of dripping, ease of removal (peel-off property), and appropriate pack strength) and excellent stability.

Claims (3)

A two-part solidification composition that gels by mixing (1) a first part and (2) a second part shown below,
(1) A first agent containing water and tamarind gum ; and (2) a second agent containing a polyhydric alcohol. The two-part solidification composition is characterized in that an alkyl acrylate copolymer is contained in at least one of the first agent and the second agent. The two-component solidifying composition according to claim 1, wherein the polyhydric alcohol contains one or more selected from glycerin, butylene glycol, dipropylene glycol, isopentyl diol, propane diol and diglycerin. The two-part solidifying composition according to claim 1 or 2 is a peel-off pack in which the first and second parts are mixed, applied to the skin to gel, and then peeled off.