JP2017088582A - Method of discriminating filling molding method in solid powder cosmetic - Google Patents

Method of discriminating filling molding method in solid powder cosmetic Download PDF

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JP2017088582A
JP2017088582A JP2015224628A JP2015224628A JP2017088582A JP 2017088582 A JP2017088582 A JP 2017088582A JP 2015224628 A JP2015224628 A JP 2015224628A JP 2015224628 A JP2015224628 A JP 2015224628A JP 2017088582 A JP2017088582 A JP 2017088582A
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stress
filling molding
solid powder
shear
molding method
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JP6601952B2 (en
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直晃 豊田
Naoaki Toyoda
直晃 豊田
浩志 浅野
Hiroshi Asano
浩志 浅野
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Nippon Menard Cosmetic Co Ltd
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Abstract

PROBLEM TO BE SOLVED: To solve the problem that discriminating between a solid powder cosmetic obtained by a wet filling molding method and that obtained by a dry filling molding method is actually impossible, because there was no means for objectively evaluating the characteristics of a solid powder cosmetic molded by a wet filling molding method which is said to have smoothness and a moisturizing feeling compared with that molded by a dry filling molding method.SOLUTION: Provided is a method of discriminating between a solid powder cosmetic molded by a wet filling molding method and that of a dry filling molding method using a shear adhesion stress τobtained from a specific powder layer shear force measurement as a physical property index.SELECTED DRAWING: Figure 1

Description

本願発明は、充填成型法の異なる固形粉末化粧料を客観的に判別する方法に関する。   The present invention relates to a method for objectively discriminating solid powder cosmetics having different filling molding methods.

メイクアップ化粧料、特に処方の大部分を粉末が占める粉末化粧料においては、製造した粉末化粧料基剤をそのままお客様へ提供することは少なく、充填成型工程を経て商品化することが一般的である。充填成型工程は商品を差別化する上で重要な要素となる。   For makeup cosmetics, especially powder cosmetics where the majority of the prescription is powder, it is rare to provide the manufactured powder cosmetic base to customers as it is, and it is common to commercialize it through a filling molding process. is there. The filling and molding process is an important factor in differentiating products.

パウダーファンデーションなどに代表される固形粉末化粧料の充填成型法は、乾式充填成型法と湿式充填成型法の二種類に分けられる。前者は、粉末化粧料基剤を直接圧縮する成型法で、後者は粉末化粧料基剤と炭化水素などの溶剤、あるいは水とを混合してスラリー化し、圧縮・乾燥させる成型法である。湿式充填成型法によって成型された固形粉末化粧料は、なめらかでしっとりとした使用感触を得られることから、ニーズの高い方法として近年広く普及している(例えば特許文献1〜10)。   Solid powder cosmetic filling and molding methods represented by powder foundations and the like can be classified into two types: dry filling molding methods and wet filling molding methods. The former is a molding method in which a powder cosmetic base is directly compressed, and the latter is a molding method in which a powder cosmetic base and a solvent such as hydrocarbon or water are mixed to form a slurry, and then compressed and dried. In recent years, solid powder cosmetics molded by a wet filling molding method have been widely spread as a method with high needs since a smooth and moist use feeling can be obtained (for example, Patent Documents 1 to 10).

それぞれの充填成型法によって得られる固形粉末化粧料は、使用感触の違いは明らかであるものの、例えば外観からその違いを判別することは出来ない。また、固形粉末化粧料の品質を保証する目的で硬度や色差といった製品規格項目を設定することが一般的であるが、これらの項目からでは湿式、及び乾式充填成型法の違いを判別できないことが多い。つまり、物性値は成型する前の固形粉末化粧料基剤の特性に大きく依存し、充填成型法の違いでは物性値には差が表れてこないものと考えられる。   The solid powder cosmetics obtained by the respective filling molding methods can clearly discriminate the difference from the appearance, for example, although the difference in the feeling of use is clear. In addition, it is common to set product standard items such as hardness and color difference for the purpose of guaranteeing the quality of solid powder cosmetics, but it is not possible to distinguish the difference between wet and dry filling molding methods from these items. Many. In other words, the physical property value largely depends on the characteristics of the solid powder cosmetic base before molding, and it is considered that no difference appears in the physical property value due to the difference in the filling molding method.

一般に、湿式充填成型法によって成型された固形粉末化粧料は、乾式充填成型法に比べて、前述したようになめらかでしっとりとした使用感触であると言われている。しかし、このような感触特性は、評価者の感性に大きく影響される主観的な指標である。つまり、湿式、及び乾式充填成型法により得られる固形粉末化粧料を判別するのは現実的に不可能な状況にある。   In general, solid powder cosmetics molded by a wet filling molding method are said to have a smooth and moist use feeling as described above compared to a dry filling molding method. However, such a touch characteristic is a subjective index greatly influenced by the evaluator's sensitivity. That is, it is practically impossible to discriminate solid powder cosmetics obtained by wet and dry filling molding methods.

これらの背景に基づき、上記不明確性を取り除くために、異なる充填成型法によって成型された固形粉末化粧料を客観的に判別し得る指標が強く望まれている。   Based on these backgrounds, in order to remove the ambiguity, an index that can objectively distinguish solid powder cosmetics molded by different filling molding methods is strongly desired.

特許第3675564号公報Japanese Patent No. 3675564 特許第5404068号公報Japanese Patent No. 5404068 特許第5432656号公報Japanese Patent No. 5432656 特許第5558061号公報Japanese Patent No. 5555861 特許第5611569号公報Japanese Patent No. 56111569 特開2002−241230号公報JP 2002-241230 A 特開2012−184211号公報JP 2012-184 211 A 特開2014−65691号公報JP 2014-65691 A 特開2014−101293号公報JP 2014-101293 A 特開2015−86156号公報JP-A-2015-86156

本願発明は、上記事情に鑑みてなされたもので、湿式、及び乾式充填成型法で成型された固形粉末化粧料を、物理機器を用いて客観的に判別するための方法を提供することを目的とする。   The present invention has been made in view of the above circumstances, and an object thereof is to provide a method for objectively discriminating solid powder cosmetics molded by wet and dry filling molding methods using physical equipment. And

かかる実情において、本願発明者らは上記課題を解決すべく鋭意研究を重ねた結果、特定の粉体層せん断力測定から得られるせん断付着応力τを物性指標として用いることで、湿式、及び乾式充填成型法で成型された固形粉末化粧料を判別出来ることを見出し、本願発明を完成するに至った。 In such a situation, the inventors of the present application have made extensive studies to solve the above problems, and as a result, by using the shear bond stress τ c obtained from a specific powder layer shear force measurement as a physical property index, a wet type and a dry type The present inventors have found that solid powder cosmetics molded by the filling molding method can be distinguished, and have completed the present invention.

すなわち本願発明は、粉末と油性成分とを混合して得られる固形粉末化粧料基剤を用いて湿式、及び乾式充填成型法で成型された各固形粉末化粧料を、特定の方法による粉体層せん断力測定(垂直応力σ、及びせん断応力τが定常状態に達した後、定容積状態にて連続的に垂直応力を減衰した時に同時に得られるせん断応力をプロットする方法)から得られるせん断付着応力τを物性指標として関連付けて判別する方法を提供するものである。 That is, the present invention relates to a powder layer formed by a specific method for each solid powder cosmetic molded by a wet and dry filling molding method using a solid powder cosmetic base obtained by mixing powder and an oil component. Shear bond stress obtained from shear force measurement (a method of plotting the shear stress obtained at the same time when normal stress σ and shear stress τ reach steady state and then continuously attenuate normal stress in constant volume state) there is provided a method for determining in association with tau c as physical indicator.

本願発明は、湿式、及び乾式充填成型法で成型された固形粉末化粧料を客観的に判別するため、特定の方法による粉体層せん断力測定から得られるせん断付着応力τを物性指標として関連付けるものである。 In the present invention, in order to objectively discriminate solid powder cosmetics molded by wet and dry filling molding methods, the shear adhesion stress τ c obtained from the powder layer shear force measurement by a specific method is related as a physical property index. Is.

粉体層せん断力測定装置概略Outline of powder bed shear force measuring device

以下本願発明の、粉末と油性成分とを混合して得られる固形粉末化粧料基剤を用いて湿式、及び乾式充填成型法で成型された各固形粉末化粧料の判別方法を、その好ましい実施形態に基づいて説明する。本願発明によれば、湿式、及び乾式充填成型法で成型された固形粉末化粧料を客観的に判別することが出来る。   Hereinafter, a preferred embodiment of a method for discriminating each solid powder cosmetic molded by a wet and dry filling molding method using a solid powder cosmetic base obtained by mixing a powder and an oily component of the present invention. Based on According to the present invention, it is possible to objectively discriminate solid powder cosmetics molded by wet and dry filling molding methods.

本願発明の固形粉末化粧料における充填成型法の判別方法は、評価の対象となる固形粉末を用いて粉体層せん断力測定を実施し、垂直応力σに対応するせん断応力τをプロットして得られるせん断付着応力τ(σ=0時のτ値)により、前記固形粉末化粧料の充填成型法を判別する。 The determination method of the filling molding method in the solid powder cosmetic of the present invention is obtained by measuring the powder layer shear force using the solid powder to be evaluated and plotting the shear stress τ corresponding to the normal stress σ. The solid powder cosmetic filling and molding method is discriminated by the shear bond stress τ c (σ value when σ = 0).

本願発明の実施形態においては、下記手順に従った粉体層せん断力測定から得られるせん断付着応力τを物性指標として評価する。
(1)円柱状のセル(上部固定セル、下部可動セル)内部に、セル内径に等しく円柱状にくり抜いた固形粉末化粧料を充填し、垂直応力を一定の速度で徐々に負荷する。
(2)垂直応力の規定値に達した後、垂直応力の負荷を停止し定容積状態で粉体層の緩和時間を設ける。
(3)十分に応力緩和が起こった後に、セルに一定速度で水平方向の外力を負荷する。
(4)せん断が定常状態(垂直応力とせん断応力の値がそれぞれ一定となる状態)に達した後、水平方向の外力を保持したまま垂直応力を徐々に減衰させていく。
(5)前記減衰過程で、垂直応力とせん断応力を検知して得られた各垂直応力σ(横軸:x軸)に対応するせん断応力τ(縦軸:y軸)をプロットし、せん断付着応力τ(σ=0時のτ値)を得る。
In the embodiment of the present invention, the shear adhesion stress τ c obtained from the powder layer shear force measurement according to the following procedure is evaluated as a physical property index.
(1) Solid powder cosmetics hollowed out in a cylindrical shape equal to the cell inner diameter are filled into cylindrical cells (upper fixed cells, lower movable cells), and vertical stress is gradually applied at a constant rate.
(2) After reaching the specified value of the normal stress, the normal stress load is stopped and a relaxation time of the powder layer is provided in a constant volume state.
(3) After sufficient stress relaxation has occurred, a horizontal external force is applied to the cell at a constant speed.
(4) After the shear reaches a steady state (a state in which the values of the vertical stress and the shear stress are constant), the vertical stress is gradually attenuated while maintaining the external force in the horizontal direction.
(5) In the damping process, the shear stress τ (vertical axis: y-axis) corresponding to each vertical stress σ (horizontal axis: x-axis) obtained by detecting the vertical stress and shear stress is plotted, and the shear adhesion Stress τ c (τ value at σ = 0) is obtained.

上記手順に従って得られた湿式充填成型品Wのせん断付着応力τ(W)と、乾式充填成型品Dのせん断付着応力τ(D)において、τ(W)>τ(D)となる。 In the shear adhesion stress τ c (W) of the wet filling molded product W obtained according to the above procedure and the shear adhesion stress τ c (D) of the dry filling molding product D, τ c (W)> τ c (D) Become.

測定を正確に行うため、湿式、及び乾式充填成型法で成型された固形粉末化粧料の判別評価では、負荷する垂直応力は、実際にセル内部の粉末を押し込んだ押し込み荷重ではなく、押し込まれたことにより粉末にかかる正味の荷重である底面荷重をロードセルで制御することが好ましい。底面荷重で検知すれば、セル壁面摩擦による圧力欠損の影響を無くし、粉体層にかかる実荷重を規定することが出来る。   In order to accurately measure, in the discrimination evaluation of solid powder cosmetics molded by wet and dry filling molding method, the vertical stress to be applied was not the indentation load that actually pushed the powder inside the cell, but was indented Thus, it is preferable to control the bottom load, which is the net load applied to the powder, by the load cell. If it is detected by the bottom surface load, it is possible to eliminate the influence of the pressure deficiency due to the cell wall friction and to define the actual load applied to the powder layer.

湿式、及び乾式充填成型法で成型された固形粉末化粧料の判別評価において、τ(W)>τ(D)であれば十分に評価判別出来るが、τ(W)/τ(D)≧1.2であればより正確に評価判別することが出来る。 In the discrimination evaluation of the solid powder cosmetics molded by the wet and dry filling molding methods, if τ c (W)> τ c (D), the evaluation can be sufficiently performed, but τ c (W) / τ c ( If D) ≧ 1.2, the evaluation can be determined more accurately.

湿式、及び乾式充填成型法で成型された固形粉末化粧料の判別評価において、円柱状セル(円柱状上部固定セル、及び円柱状下部可動セル)の内径は、特に限定されないが3〜43mmの範囲であることが好ましい。円柱状セルの内径が3mm以下では、せん断時に適切な粉体層面積を保持出来ない場合があり、43mm以上では使用するサンプル量が増える上、粉体層面積の保持に関してそれ以上の効果は見込めない。   In the discrimination evaluation of the solid powder cosmetics molded by the wet and dry filling molding methods, the inner diameter of the columnar cells (columnar upper fixed cell and columnar lower movable cell) is not particularly limited, but is in the range of 3 to 43 mm. It is preferable that If the inner diameter of the cylindrical cell is 3 mm or less, an appropriate powder layer area may not be maintained during shearing. If it is 43 mm or more, the amount of sample to be used increases, and further effects on the maintenance of the powder layer area can be expected. Absent.

湿式、及び乾式充填成型法で成型された固形粉末化粧料の判別評価において、円柱状下部可動セルの深さは、特に限定されないが1〜5mmの範囲であることが好ましい。円柱状下部可動セルの深さが1mm以下では、せん断時に適切な粉体層面積を保持出来ない場合があり、5mm以上では使用するサンプル量が増える上、粉体層面積の保持に関してそれ以上の効果は見込めない。   In the discrimination evaluation of solid powder cosmetics molded by wet and dry filling molding methods, the depth of the columnar lower movable cell is not particularly limited but is preferably in the range of 1 to 5 mm. If the depth of the cylindrical lower movable cell is 1 mm or less, an appropriate powder layer area may not be maintained at the time of shearing. If the depth is 5 mm or more, the amount of sample to be used increases and the powder layer area is further maintained. The effect is not expected.

湿式、及び乾式充填成型法で成型された固形粉末化粧料の判別評価において、手順(1)で負荷する垂直応力の規定値は、特に限定されないが100〜1100kPaの範囲であることが好ましい。垂直応力が100kPa以下では粉体層の形成が十分でない場合がある。垂直応力が1100kPa以下であれば、粉体層の形成が十分に行われる。   In the discrimination evaluation of the solid powder cosmetics molded by the wet and dry filling molding methods, the specified value of the vertical stress applied in the procedure (1) is not particularly limited, but is preferably in the range of 100 to 1100 kPa. When the normal stress is 100 kPa or less, the powder layer may not be sufficiently formed. If the normal stress is 1100 kPa or less, the powder layer is sufficiently formed.

湿式、及び乾式充填成型法で成型された固形粉末化粧料の判別評価において、手順(2)で設ける緩和時間は、特に限定されないが50〜100secの範囲であることが好ましい。緩和時間が50sec以下では、応力緩和が十分でない場合があり、正確な測定が出来ない場合がある。緩和時間が100sec以下であれば、十分な応力緩和を得ることが出来る。   In the discrimination evaluation of the solid powder cosmetics molded by the wet and dry filling molding methods, the relaxation time provided in the procedure (2) is not particularly limited, but is preferably in the range of 50 to 100 sec. If the relaxation time is 50 sec or less, stress relaxation may not be sufficient, and accurate measurement may not be possible. If the relaxation time is 100 sec or less, sufficient stress relaxation can be obtained.

湿式、及び乾式充填成型法で成型された固形粉末化粧料の判別評価において、手順(3)で負荷する水平方向の外力の進行速度は、特に限定されないが10〜100μm/secの範囲であることが好ましい。進行速度が100μm/sec以上では、せん断速度が速すぎて適切な粉体層面積を保持出来ず正確な測定が出来ない場合がある。速度が10μm/sec以上であれば、適切な粉体層面積を十分保持したまま効率良く粉体層をせん断出来る。   In the discrimination evaluation of solid powder cosmetics molded by wet and dry filling molding methods, the speed of progression of the external force applied in the horizontal direction in step (3) is not particularly limited, but is in the range of 10 to 100 μm / sec. Is preferred. When the traveling speed is 100 μm / sec or more, there are cases where the shear rate is too high to maintain an appropriate powder layer area and accurate measurement cannot be performed. If the speed is 10 μm / sec or more, the powder layer can be efficiently sheared while maintaining an adequate powder layer area.

湿式、及び乾式充填成型法で成型された固形粉末化粧料の判別評価において、粉体層せん断帯厚み(円柱状上部固定セルと円柱状下部可動セルの間隙)は、特に限定されないが0.1〜0.3mmの範囲であることが好ましい。粉体層せん断帯厚みが0.3mm以上では、一定の粉体層せん断帯を保持したまません断出来ない場合があり、0.1mm以下では粉体層せん断帯の保持に関してそれ以上の効果は見込めない。   In the discrimination evaluation of the solid powder cosmetics molded by the wet and dry filling molding methods, the thickness of the powder layer shear zone (the gap between the cylindrical upper fixed cell and the cylindrical lower movable cell) is not particularly limited, but 0.1 It is preferable to be in the range of ~ 0.3 mm. If the thickness of the powder layer shear band is 0.3 mm or more, it may not be possible to shear while maintaining a certain powder layer shear band. If the thickness is 0.1 mm or less, further effects on the retention of the powder layer shear band can be expected. Absent.

湿式、及び乾式充填成型法で成型された固形粉末化粧料の判別評価において、各応力のデータ取り込み間隔は、特に限定されないが1〜500msecの範囲であることが好ましい。データ取り込み間隔が500msec以上では、十分なプロット数が得られない場合がある。データ取り込み間隔が1msec以上であれば、十分なプロット数を得ることが出来る。   In the discrimination evaluation of solid powder cosmetics molded by wet and dry filling molding methods, the data acquisition interval of each stress is not particularly limited, but is preferably in the range of 1 to 500 msec. When the data capture interval is 500 msec or more, there are cases where a sufficient number of plots cannot be obtained. If the data capture interval is 1 msec or more, a sufficient number of plots can be obtained.

せん断付着応力τは、図1に示すような粉体層せん断力測定装置を用いて測定出来る。この装置では、前述のように垂直応力を底面荷重で検知しているのが特徴である。本装置以外にも例えば、市販品である粉体層せん断力測定装置NS−S500(ナノシーズ社製)を用いても測定出来る。粉体層せん断力測定を実施する時の室内温度及び相対湿度は、化粧料使用時の環境を考慮すると、10〜35℃、及び30〜65%RHが好ましい。 The shear adhesion stress τ c can be measured using a powder layer shear force measuring apparatus as shown in FIG. As described above, this apparatus is characterized in that the vertical stress is detected by the bottom load. In addition to this apparatus, for example, measurement can also be performed using a commercially available powder layer shear force measuring apparatus NS-S500 (manufactured by Nano Seeds). The room temperature and relative humidity when the powder layer shear force measurement is performed are preferably 10 to 35 ° C. and 30 to 65% RH in consideration of the environment when the cosmetic is used.

以下実施例により本願発明をさらに詳細に説明する。尚、これらは本願発明を何ら限定するものではない。   Hereinafter, the present invention will be described in more detail with reference to examples. In addition, these do not limit this invention at all.

(実施例1)
表1に示す処方の固形粉末化粧料基剤を下記製造方法に従い調製し、湿式充填成型、及び乾式充填成型によって得られたパウダーファンデーションについて、下記のようにして粉体層せん断力測定を実施して、せん断付着応力τを得た。
測定装置:粉体層せん断力測定装置(ナノシーズ社製 試作機)
測定条件:室内温度25℃、相対湿度50%RH
円柱状上部固定セル(内径15mm)
円柱状下部可動セル(深さ1mm)
粉体層せん断帯厚み0.2mm
垂直方向進行速度200μm/sec
水平方向進行速度10μm/sec
データ取り込み間隔100msec
手順(1)で負荷した初期垂直応力1000kPa
Example 1
A solid powder cosmetic base having the formulation shown in Table 1 was prepared according to the following manufacturing method, and the powder layer shear force was measured as follows for the powder foundation obtained by wet filling molding and dry filling molding. Thus, a shear bond stress τ c was obtained.
Measuring device: Powder layer shear force measuring device (prototype manufactured by Nano Seeds)
Measurement conditions: indoor temperature 25 ° C., relative humidity 50% RH
Cylindrical upper fixed cell (inner diameter 15mm)
Cylindrical lower movable cell (depth 1mm)
Powder layer shear zone thickness 0.2mm
Vertical traveling speed 200μm / sec
Horizontal traveling speed 10μm / sec
Data capture interval 100msec
Initial vertical stress of 1000 kPa applied in step (1)

(表1)
(Table 1)

(製造方法)
成分1〜15をヘンシェルミキサーにて均一に混合し、アトマイザーにて粉砕を行った。さらに、成分1〜15の混合粉砕物と、予め加熱混合しておいた成分16〜19をヘンシェルミキサーに加えて均一に混合し、アトマイザー粉砕後、ふるいを通して固形粉末化粧料基剤を得た。
(Production method)
Ingredients 1 to 15 were uniformly mixed with a Henschel mixer, and pulverized with an atomizer. Furthermore, the mixed pulverized product of components 1 to 15 and components 16 to 19 previously heated and mixed were added to a Henschel mixer and mixed uniformly. After pulverizing the atomizer, a solid powder cosmetic base was obtained through a sieve.

(湿式充填成型)
調製した固形粉末化粧料基剤に10重量%エタノール水溶液を加え、均一混合して適度な流動性のあるスラリーをつくる。これを中皿に充填し、多孔質吸引ヘッドを用いて吸引圧縮成型する。その後、成型物を70℃で10時間乾燥して、パウダーファンデーションWを得た。尚、処方例1、及び2で得られたパウダーファンデーションはそれぞれW1、W2とした。
(Wet filling molding)
A 10% by weight ethanol aqueous solution is added to the prepared solid powder cosmetic base, and mixed uniformly to form a slurry with appropriate fluidity. This is filled in an intermediate dish and suction compression molded using a porous suction head. Thereafter, the molded product was dried at 70 ° C. for 10 hours to obtain a powder foundation W. Note that the powder foundations obtained in Formulation Examples 1 and 2 were W1 and W2, respectively.

(乾式充填成型)
調製した固形粉末化粧料基剤を中皿に充填し、圧縮成型することでパウダーファンデーションDを得た。尚、処方例1、及び2で得られたパウダーファンデーションはそれぞれD1、D2とした。
(Dry filling molding)
Powder foundation D was obtained by filling the prepared solid powder cosmetic base into an inner dish and compression molding. In addition, the powder foundations obtained in Formulation Examples 1 and 2 were D1 and D2, respectively.

下記表2に示すように処方例1、及び2のいずれにおいても、湿式充填成型法によって得られたパウダーファンデーションWは、乾式充填成型法によって得られたパウダーファンデーションDに比べてせん断付着応力τが大きく、かつτ(W)/τ(D)≧1.2となり、その充填成型法による違いを正確に評価出来ている。 As shown in Table 2 below, in each of Formulation Examples 1 and 2, the powder foundation W obtained by the wet filling molding method has a shear adhesion stress τ c as compared with the powder foundation D obtained by the dry filling molding method. And τ c (W) / τ c (D) ≧ 1.2, and the difference due to the filling molding method can be accurately evaluated.

(表2)
(Table 2)

本願発明の評価方法は、湿式、及び乾式充填成型法で成型された固形粉末化粧料を、粉体層せん断力測定から得られるせん断付着応力τを物性指標として関連付けて判別出来るものである。本願発明の評価方法によれば、従来、主観的評価法でしか評価出来なかった充填成型法の異なる固形粉末化粧料を、客観的評価に基づく物性値を用いることで特定することが出来る。 The evaluation method of the present invention can discriminate solid powder cosmetics molded by wet and dry filling molding methods by associating the shear adhesion stress τ c obtained from the powder layer shear force measurement as a physical property index. According to the evaluation method of the present invention, conventionally, solid powder cosmetics with different filling molding methods that could only be evaluated by a subjective evaluation method can be specified by using physical property values based on objective evaluation.

Claims (4)

粉末と油性成分とを混合して得られる固形粉末化粧料基剤を、湿式充填成型法、及び乾式充填成型法により成型した時、それぞれ得られた固形粉末化粧料W、及びDにおいて、下記手順に従った粉体層せん断力測定から得られるせん断付着応力τを物性指標として評価判別する方法。
(1)円柱状のセル(上部固定セル、下部可動セル)内部に、セル内径に等しく円柱状にくり抜いた前記固形粉末化粧料を充填し、垂直応力を一定の速度で徐々に負荷する。
(2)垂直応力の規定値に達した後、垂直応力の負荷を停止し定容積状態で粉体層の緩和時間を設ける。
(3)十分に応力緩和が起こった後に、セルに一定速度で水平方向の外力を負荷する。
(4)せん断が定常状態(垂直応力とせん断応力の値がそれぞれ一定となる状態)に達した後、水平方向の外力を保持したまま垂直応力を徐々に減衰させていく。
(5)前記減衰過程で、垂直応力とせん断応力を検知して得られた各垂直応力σ(横軸:x軸)に対応するせん断応力τ(縦軸:y軸)をプロットし、せん断付着応力τ(σ=0時のτ値)を得る。
When solid powder cosmetic base obtained by mixing powder and oil component is molded by wet filling molding method and dry filling molding method, in the obtained solid powder cosmetics W and D, respectively, A method for evaluating and discriminating the shear adhesion stress τ c obtained from the measurement of the shear force of the powder layer in accordance with the physical property index.
(1) Fill the cylindrical cell (upper fixed cell, lower movable cell) with the solid powder cosmetic material hollowed out in a cylindrical shape equal to the cell inner diameter, and gradually apply vertical stress at a constant rate.
(2) After reaching the specified value of the normal stress, the normal stress load is stopped and a relaxation time of the powder layer is provided in a constant volume state.
(3) After sufficient stress relaxation has occurred, a horizontal external force is applied to the cell at a constant speed.
(4) After the shear reaches a steady state (a state in which the values of the vertical stress and the shear stress are constant), the vertical stress is gradually attenuated while maintaining the external force in the horizontal direction.
(5) In the damping process, the shear stress τ (vertical axis: y-axis) corresponding to each vertical stress σ (horizontal axis: x-axis) obtained by detecting the vertical stress and shear stress is plotted, and the shear adhesion Stress τ c (τ value at σ = 0) is obtained.
湿式充填成型法によって成型した固形粉末化粧料のせん断付着応力τ(W)と、乾式充填成型法によって成型した固形粉末化粧料のせん断付着応力τ(D)とを比較した時、τ(W)>τ(D)となることを特徴とする請求項1記載の評価判別方法。 When comparing the shear adhesion stress τ c (W) of the solid powder cosmetic molded by the wet filling molding method with the shear adhesion stress τ c (D) of the solid powder cosmetic molded by the dry filling molding method, τ c The evaluation determination method according to claim 1, wherein (W)> τ c (D). τ(W)/τ(D)≧1.2であることを特徴とする請求項1又は2記載の評価判別方法。 The evaluation discrimination method according to claim 1, wherein τ c (W) / τ c (D) ≧ 1.2. 前記手順の(1)で負荷する垂直応力の範囲が、100〜1100kPaであることを特徴とする請求項1〜3のいずれか一項記載の評価判別方法。
The evaluation discrimination method according to any one of claims 1 to 3, wherein a range of the vertical stress applied in (1) of the procedure is 100 to 1100 kPa.
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