KR101133067B1 - Cosmetic formulation of a W/O/W multiple emulsion containing olive oil by one-step process - Google Patents
Cosmetic formulation of a W/O/W multiple emulsion containing olive oil by one-step process Download PDFInfo
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Abstract
본 발명은 피부에 안전한 올리브 오일을 이용한 유화물 중에서 W/O/W 형태의 다중 유화물을 단일 공정으로 제조할 수 있는 화장품 조성물에 관한 것이다. 기존의 W/O/W 형태의 다중 유화물 제조 시에는 제조시간이 길고 제형 안정성이 낮은 단점이 있다. 이에 반해 본 발명의 화장료 조성물은 기존의 제조방법이 가지고 있는 단점을 극복한 단일공정으로 일반적인 O/W 형태의 유화물과 제조시간이 동일하면서 제형 안정성이 우수한 화장료 조성물을 얻을 수 있다.The present invention relates to a cosmetic composition capable of producing multiple emulsions in the form of W / O / W in an emulsion using olive oil which is safe for skin. In the conventional production of multiple emulsions of W / O / W type, there is a disadvantage in that the preparation time is long and the formulation stability is low. On the contrary, the cosmetic composition of the present invention can obtain a cosmetic composition having excellent formulation stability while having the same manufacturing time as an emulsion of a general O / W form in a single process that overcomes the disadvantages of the conventional manufacturing method.
W/O/W 다중 유화물, 단일 공정, 올리브 오일, 화장료 W / O / W multiple emulsions, single process, olive oil, cosmetics
Description
도 1은 본 발명의 실시예에 의해 제조한 유화물 중 하나의 현미경 사진이다.1 is a micrograph of one of the emulsions prepared by an embodiment of the present invention.
본 발명은 올리브 오일을 이용하여 W/O/W 다중 유화물(multiple emulsion)을 제조함에 있어서 단일 공정 제조를 가능하게 하는 원료를 혼합한 화장료 조성물에 관한 것이다. The present invention relates to a cosmetic composition in which raw materials are mixed to enable a single process production in preparing W / O / W multiple emulsions using olive oil.
기존의 다중 유화물의 제조는 제1공정으로 W/O 유화물을 제조하여 안정화시킨 후 제2공정으로 W/O 유화물을 수상에 분산시켜 최종 유화물을 얻는 방법이 일반적이다. 그러나 이 경우 제조시간이 길어져 에너지 손실이 크고 제조 방법이 복잡하며 단순 O/W 유화물에 비해 많은 계면활성제와 원료의 사용이 불가피하여 피부 안전성이 저해되는 단점을 가지고 있다. 또한 제조된 다중 유화물은 장기적으로 안정화된 제형을 얻기가 힘들어 개발에 한계점을 가지고 있다. 본 발명의 화장료 조성물은 이러한 단점들을 극복하기 위해 단일 공정으로 제조하며 왁스와 점증제의 사용으로 제형 안정성이 우수한 W/O/W 다중 유화물을 얻을 수 있다.In the conventional production of multiple emulsions, a method of preparing and stabilizing a W / O emulsion in a first step is generally followed by dispersing the W / O emulsion in an aqueous phase in a second step to obtain a final emulsion. However, in this case, the manufacturing time is long, the energy loss is large, the manufacturing method is complicated, and the use of many surfactants and raw materials is inevitable compared to simple O / W emulsions, and thus the skin safety is impaired. In addition, the prepared multiple emulsions have limitations in development since it is difficult to obtain a long-term stabilized formulation. The cosmetic composition of the present invention can be produced in a single process to overcome these disadvantages and can be obtained W / O / W multiple emulsion with excellent formulation stability by the use of waxes and thickeners.
다중 유화물은 유화물 내 유화물로서 분산상의 입자들이 그보다 더 작은 분산 입자들을 가지고 있는 형태이다. 이러한 다중 유화물은 W/O 유화물의 보습효과와 O/W 유화물의 산뜻한 사용감을 모두 가지고 있으며, 내부 수상에 용해된 유효성분의 지속적인 방출제어가 가능하고, 내부 수상과 외부수상에 서로 다른 유효성분을 사용할 수 있으면서 유효 성분으로 인한 자극이 완화되는 장점을 가지고 있다. 이러한 이유로 다중 유화물은 식품, 화장품, 의약 분야에서 많이 응용되고 있다. Multiple emulsions are emulsions in emulsions in which the dispersed phase particles have smaller dispersed particles. These multiple emulsions have both the moisturizing effect of the W / O emulsion and the refreshing feel of the O / W emulsion, and enable continuous release control of the active ingredient dissolved in the inner water phase, and provide different active ingredients in the inner and outer water phases. While it can be used, it has the advantage that the irritation caused by the active ingredient is alleviated. For this reason, multiple emulsions are widely used in food, cosmetics and medicine.
다중 유화물은 단일 공정이나 총 2단계 공정으로 제조될 수 있다. 기존의 단일 공정에 의한 제조는 D상 유화법이나 PIT(Phase Inversion Temperature) 유화법에 의한 것이 있지만 두 경우 모두 재현성이 부족하여 응용이 제한되어 있다. 또한 총 2단계 공정으로 제조된 다중 유화물이라 할지라도 크고 다중 분산된 입자들이 열역학적으로 불안정하여 오일성 막을 통해 내수상이 단순하게 확산되거나 오일성 필름의 붕괴에 의해 내수상 입자들이 외수상으로 이동하여 입자들끼리 응집되고 합일되며 크리밍 되려는 경향을 강하게 나타내기 때문에 일반 유화물에 비해 불안정하다. 이러한 문제점들로 인해 안정한 다중 유화물의 제조가 제한되고 있으며 특히 단일 공정의 경우에는 체계적인 연구가 부족하여 장기적으로 안정해야 하는 상업적인 제품으로의 응용에 많은 제약이 따르고 있다.Multiple emulsions can be produced in a single process or a total of two stages. Existing single processes are prepared by D phase emulsification or PIT (Phase Inversion Temperature) emulsification, but both have limited reproducibility and limited applications. In addition, even in the case of multiple emulsions produced in a total two-step process, large and multi-dispersed particles are thermodynamically unstable, so that the aqueous phase simply diffuses through the oily membrane or the aqueous phase particles move to the external phase due to the collapse of the oily film. It is unstable compared to general emulsions because it strongly indicates the tendency to aggregate, coalesce and cream together. Due to these problems, the production of stable multi-emulsions is limited, and in particular, a single process has a lot of limitations in the application to commercial products that need to be stable in the long term due to lack of systematic research.
따라서 이러한 단점을 완화시키기 위해 외수상에 점증제를 첨가하여 입자들 간 응집 및 합일을 막아 안정성을 높이는 방법이 일반적으로 사용되고 있다. 대한민국 특허출원 2003-0032699호(공개번호 2004-100394호)에서는 오일로서 디메치콘, 세틸 옥타노에이트를 사용하고 또한 점증제로 카보머를 사용하여 25도, 37도 및 45도에서 1개월간 안정한 W/O/W 다중 유화물을 단일공정으로 제조하였으며, 대한민국 특허출원 2001-0077151호(공개번호2003-464863호)에서는 오일로서 카프릴릭/카프릭트리 글레세라이드를 사용하고 또한 점증제를 사용하여 안정한 다중유화물을 제조하였다. 그러나 이들 특허의 다중 유화물에서는 W/O 입자의 안정성이 낮으면 내수상 입자들 간 합일에 의해 하나의 큰 입자가 형성되어 상품 가치를 떨어뜨리고 또한 외수상으로의 확산으로 인해 W/O/W 다중 유화물의 안정성이 낮아지게 된다. 이러한 현상을 막기 위해서는 유화제를 더 첨가하여 유상-수상 계면 막을 강화해야 하는데 이 경우 피부 안전성이 낮아지게 되는 문제점이 있다.Therefore, in order to alleviate this disadvantage, a method of increasing stability by adding a thickener to the external water to prevent aggregation and coalescence between particles is generally used. Korean Patent Application No. 2003-0032699 (Publication No. 2004-100394) uses dimethicone, cetyl octanoate as oil and carbomer as a thickener, and stabilizes W / A at 25 °, 37 ° and 45 ° for 1 month. O / W multiple emulsions were prepared in a single process, and Korean Patent Application No. 2001-0077151 (Publication No. 2003-464863) uses caprylic / caprictri glycerides as oils and is also stable using multiple thickeners. An emulsion was prepared. However, in the multiple emulsions of these patents, when the stability of the W / O particles is low, one large particle is formed by coalescence between the water-in-water particles, resulting in a loss of commodity value and also due to diffusion into the outer water phase. The stability of the emulsion becomes low. In order to prevent this phenomenon, it is necessary to reinforce the oil-water interface membrane by adding an emulsifier, in which case there is a problem that the skin safety is lowered.
이상과 같은 문제점을 고려하여, 본 발명에서는 기존의 다중 유화물 제조방법이 갖는 한계를 극복하면서 다중 유화물이 갖는 장점을 강화한 단일 공정에 의한 제조방법으로, 올리브 오일을 사용하여 피부안정성을 높이고, 왁스로 유상의 안정성을 향상시키며 점증제로 외수상의 점도를 증가시켜 장기 제형 안정성을 향상시킨 화장료 조성물을 제공하고자 하는 것을 목적으로 한다.In view of the above problems, the present invention is a manufacturing method by a single process that enhances the advantages of the multiple emulsion while overcoming the limitations of the conventional multiple emulsion production method, using olive oil to increase skin stability, wax An object of the present invention is to provide a cosmetic composition which improves stability of an oil phase and improves long-term formulation stability by increasing the viscosity of an external aqueous phase with a thickener.
상기 목적을 달성하기 위하여 본 발명은 W/O/W 다중 유화물을 단일공정으로 제조 가능한 조성물로서, 원료중 유화제가 폴리글리세릴-40 스테아레이트 0.2 내지 5 중량%, 소르비탄 세스퀴올레이트 0.2 내지 5 중량 %, 글리세릴 스테아레이트 0.1 내지 5 중량 %, 폴리글리세릴-30 디폴리하이드록시스테아레이트 0.1 내지 2 중량 %, 지방산으로 정제 스테아린산 0.1 내지 5 중량 %, 왁스 0.5 내지 10 중량 %, 올리브 오일 1 내지 20 중량 %, 및 점증제 0.02 내지 5 중량 %를 함유하는 것을 특징으로 하는 W/O/W 다중 유화 조성물을 제공한다.In order to achieve the above object, the present invention provides a composition capable of producing a W / O / W multiple emulsion in a single process, the emulsifier in the raw material is 0.2 to 5% by weight of polyglyceryl-40 stearate, 0.2 to 5 sorbitan sesquioleate % By weight, glyceryl stearate 0.1-5%, polyglyceryl-30 dipolyhydroxystearate 0.1-2% by weight, 0.1-5% by weight stearic acid purified with fatty acids, 0.5-10% by weight wax, olive oil 1 To 20% by weight, and 0.02 to 5% by weight thickener is provided.
폴리글리세릴-40 스테아레이트와 소르비탄세스퀴올레이트를 0.2 중량% 미만 사용하는 경우와 글리세릴스테아레이트와 폴리글리세릴-30 디폴리하이드록시스테아레이트를 0.1 중량% 미만으로 사용하는 경우에는 내수상-유상 계면 혹은 유상-외수상 계면에 계면활성제가 충분히 배열하지 못하게 되어 장기적인 제형 안정성이 낮아지게 되거나 W/O/W 다중 유화물이 불완전하게 생성되거나 또는 생성되지 않는다. 폴리글리세릴-40 스테아레이트와 소르비탄 세스퀴올레이트 및 글리세릴 스테아레이트를 5 중량% 이상 사용하는 경우와 폴리글리세릴-30 디폴리하이드록시스테아레이트를 2 중량% 이상으로 사용하는 경우에는 원료가 석출되거나 W/O/W 다중 유화물이 불완전하게 생성 또는 생성되지 않는다. 정제 스테아린산을 0.1 중량% 미만으로 사용하는 경우에는 제형 안정성을 높이는데 효과가 없으며, 5 중량% 이상 사용하는 경우에는 W/O/W 다중 유화물이 생성되지 않거나 불완전하게 생성되고 장기 제형 안정성도 낮아지게 된다. 왁스를 0.5 중량% 미만으로 사용하는 경우에는 제형 안정성을 높이는 효과를 나타내지 못하며 10 중량% 이상으로 사용하는 경우에는 오히려 제형 안정성을 낮게 하며, 올리브 오일을 1 중량% 미만 또는 20 중량% 이상으로 사용하는 경우에는 W/O/W 다중 유화물이 생성되지 않는다. 점증제를 0.02 중량% 미만으로 사용하는 경우에는 점증되지 않고 제형 안정성을 높여주지 못하며, 5 중량% 이상으로 사용하면 사용감 측면에서 끈적이며 흡수가 늦어 화장료로서의 상품가치 가 떨어진다. When using less than 0.2% by weight of polyglyceryl-40 stearate and sorbitassesquioleate and less than 0.1% by weight of glyceryl stearate and polyglyceryl-30 dipolyhydroxystearate Insufficient alignment of surfactants at the oil phase or oil phase-out-water interface results in low long-term formulation stability or incomplete or no W / O / W multiple emulsions. Raw materials may be used when at least 5% by weight of polyglyceryl-40 stearate and sorbitan sesquioleate and glyceryl stearate are used and when at least 2% by weight of polyglyceryl-30 dipolyhydroxystearate is used. Precipitates or W / O / W multiple emulsions are not incompletely produced or produced. The use of purified stearic acid at less than 0.1% by weight is not effective in increasing formulation stability, and when used at 5% by weight or more, W / O / W multiple emulsions are not produced or incompletely produced and the long-term formulation stability is also lowered. do. If the wax is used in less than 0.5% by weight does not show the effect of increasing the formulation stability, when used in more than 10% by weight rather lower the formulation stability, using less than 1% or 20% by weight of olive oil In this case, no W / O / W multiple emulsions are produced. If the thickener is used at less than 0.02% by weight, it does not increase and the formulation stability is not enhanced. If the thickener is used at more than 5% by weight, the product value as a cosmetic is low due to stickiness and late absorption.
본 발명의 다중 유화조성물에서 사용되는 왁스는 비즈 왁스(Bees wax), 마이크로크리스탈린 왁스(Microcrystalline wax), 파라핀 왁스, 칸데릴라 왁스(Candelilla wax) 중에서 선택된 1종 또는 2종 이상을 포함할 수 있다,The wax used in the multiple emulsion composition of the present invention may include one or two or more selected from bees wax, microcrystalline wax, paraffin wax, candelilla wax. ,
본 발명에서 점증제로는 카보머(Carbomer), 아크릴레이트/C10-30 알킬 아크릴레이트 코폴리머(Acrylates/C10-30 알킬아크리레이트 폴리머), 암모늄 아크릴롤디메틸타우레이트/비닐피롤리딘 코폴리머(Ammonium acryloyldimethyltaurate/VP copolymer), 하이드록시프로필 스타치 포스페이트(Hydroxypropyl starch phosphate), 타피오카 스타치(Tapioca starch), 잔탄검, 겔란검(Gellan gum), 하이드록시에틸셀룰로즈, 소듐 폴리아크릴레이트 중에서 선택된 1종 혹은 2종 이상을 혼합하여 사용할 수 있다.Thickeners in the present invention include carbomer, acrylate / C10-30 alkyl acrylate copolymer (Acrylates / C10-30 alkyl acrylate polymer), ammonium acrylol dimethyl taurate / vinylpyrrolidine copolymer ( 1 type selected from ammonium acryloyldimethyltaurate / VP copolymer, hydroxypropyl starch phosphate, tapioca starch, xanthan gum, gellan gum, hydroxyethylcellulose, sodium polyacrylate Or it can mix and use 2 or more types.
상기 처방에 따른 다중 유화물의 제조과정은 다음과 같다. 먼저 유화제 조합과 지방산, 왁스 및 오일 등으로 구성된 유상부와 점증제를 함유한 수상부를 70 내지 80도에서 각각 용해하고 균일하게 혼합한 다음 수상부를 패들믹서(Paddle mixer) 15 내지 50 rpm으로 서서히 교반하면서 유상부를 투입한 후 호모믹서로 1000 내지 6000 rpm으로 3 내지 10분간 유화하고 냉각하여 W/O/W 형태의 다중 유화물을 얻는다.The manufacturing process of the multiple emulsion according to the said prescription is as follows. First, the oil phase part composed of an emulsifier combination, fatty acid, wax and oil, etc. and the water phase part including the thickener are dissolved and uniformly mixed at 70-80 degrees, respectively, and then the water phase part is slowly stirred at 15 to 50 rpm with a paddle mixer. After the oil phase is added, the emulsion is emulsified for 3 to 10 minutes at 1000 to 6000 rpm using a homomixer and cooled to obtain a multiple emulsion in the form of W / O / W.
또는 점증제를 제외한 수상부와 유화제 조합과 지방산, 왁스 및 오일 등으로 구성된 유상부를 70 내지 80도로 각각 용해하고 균일하게 혼합하고 수상부를 패들믹서(Paddle mixer) 15 내지 50 rpm으로 서서히 교반하면서 유상부를 투입한 후 호 모믹서로 1000 내지 6000 rpm으로 약 3 내지 10분간 유화하고 점증제를 투입한 후 호모믹서로 1000 내지 6000rpm으로 약 3 내지 10분간 혼합한 후 냉각하여 W/O/W 형태의 다중 유화물을 얻는다.Alternatively, the oil phase portion, which is composed of an aqueous phase, an emulsifier combination, fatty acid, wax, and oil, etc., except for a thickener, is dissolved at 70 to 80 degrees, respectively, and uniformly mixed, and the oil phase is gradually stirred with a paddle mixer 15 to 50 rpm. After the addition, emulsify for about 3 to 10 minutes at 1000 to 6000 rpm with a homomixer and add a thickener, and then mix at about 3 to 10 minutes at 1000 to 6000 rpm with a homomixer, and then cool and multiply in the form of W / O / W. Get an emulsion
이하, 실시예 및 시험예에 의거하여 본 발명을 더욱 구체적으로 설명한다. 그러나 이들 실시예 및 시험예는 본 발명을 예시하는 것일 뿐, 본 발명의 기술적 범위가 이들만으로 한정되는 것은 아니다.Hereinafter, the present invention will be described in more detail based on Examples and Test Examples. However, these Examples and Test Examples are merely to illustrate the invention, the technical scope of the present invention is not limited to these.
실시예 및 비교예Examples and Comparative Examples
다음 표 1의 처방을 가지고 상기의 방법에 따라 제조하였으며, 실시예에 의해 제조한 유화물 중 하나의 현미경 사진을 도 1로 나타내었고, 장기 안정성은 이하의 평가방법 및 평가기준으로 평가했다.It was prepared according to the method described above with the prescription of Table 1, one of the photomicrographs of the emulsion prepared according to the embodiment is shown in Figure 1, the long-term stability was evaluated by the following evaluation method and evaluation criteria.
<안정성 평가방법><Stability Evaluation Method>
실시예 3과 비교예 1, 2를 25도, 37도, 45도 항온조에 3개월간 보관하여 현미경으로 관찰한다(표 2).Example 3 and Comparative Examples 1 and 2 were stored in a 25 degree, 37 degree and 45 degree incubator for 3 months and observed under a microscope (Table 2).
O : 제조 직후와 동일한 다중 유화물 상태이다.O: The same state of multiple emulsions as immediately after preparation.
△ : 다중 유화물 상태이나 내수상이 없는 유상입자를 볼 수 있다.(Triangle | delta): The oily particle which is a state of multiple emulsions or a water-resistant phase can be seen.
X : 다중 유화물 상태가 아니다.X: Not in a multiple emulsion state.
본 발명에 따른 W/O/W 형태의 다중 유화물의 단일공정 제조는 총 2단계 공정에 의한 기존의 제조방법에 비해 시간과 비용이 크게 절감되며, 왁스와 점증제의 사용으로 제형의 장기적인 안정성을 획기적으로 높임으로서 상업적인 제품생산의 걸림돌을 제거하고, 올리브오일을 사용함으로 피부안전성을 높여 일반 유화물보다 뛰어난 심리적 만족감도 얻을 수 있다. 따라서 본 발명의 화장료 조성물에 의한 W/O/W 형태의 다중 유화물의 제조기술은 상업적인 제품 생산에 획기적인 돌파구를 마련할 것으로 사료된다. The single-step manufacturing of the multi-emulsion of the W / O / W type according to the present invention significantly reduces the time and cost compared to the conventional manufacturing method by a total of two steps, and improves the long-term stability of the formulation by using waxes and thickeners. By dramatically increasing the barriers to commercial product production and using olive oil, skin safety can be improved and psychological satisfaction can be obtained better than general emulsions. Therefore, the production technology of the multi-emulsion of the W / O / W form by the cosmetic composition of the present invention is expected to provide a breakthrough breakthrough in commercial product production.
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