KR102026995B1 - Manufacturing method of solubilized petrolatum cosmetic composition - Google Patents

Manufacturing method of solubilized petrolatum cosmetic composition Download PDF

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KR102026995B1
KR102026995B1 KR1020190030786A KR20190030786A KR102026995B1 KR 102026995 B1 KR102026995 B1 KR 102026995B1 KR 1020190030786 A KR1020190030786 A KR 1020190030786A KR 20190030786 A KR20190030786 A KR 20190030786A KR 102026995 B1 KR102026995 B1 KR 102026995B1
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weight
homogenizer
minutes
petrolatum
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신복철
장시헌
허준원
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에이앤에이치 인터내셔널 코스메틱스
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/31Hydrocarbons
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/342Alcohols having more than seven atoms in an unbroken chain
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/345Alcohols containing more than one hydroxy group
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/737Galactomannans, e.g. guar; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/8141Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • A61K8/8152Homopolymers or copolymers of esters, e.g. (meth)acrylic acid esters; Compositions of derivatives of such polymers
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/49Solubiliser, Solubilising system

Abstract

The present invention relates to a method for producing a water-soluble petrolatum cosmetic composition, which comprises: a first step of heating and stirring a mixture; a second step of inputting octyldodecanol to a resultant of the first step, and stirring the same; a third step of inputting sodium polyacrylate to a resultant of the second step, and stirring the same; and a fourth step of cooling a resultant of the third step, and then inputting, stirring and cooling 1, 2-hexanediol.

Description

수용화가 가능한 페트롤라툼 화장료 조성물의 제조방법{MANUFACTURING METHOD OF SOLUBILIZED PETROLATUM COSMETIC COMPOSITION}MANUFACTURING METHOD OF SOLUBILIZED PETROLATUM COSMETIC COMPOSITION}

본 발명은 수용화가 가능한 페트롤라툼 화장료 조성물에 관한 발명이다. The present invention relates to a petrolatum cosmetic composition capable of water solubility.

페트롤라툼(바세린) 화장품은 퍼스널케어 및 화장품원료로서 수분증발차단제, 피부보호제 등 매우 유의미한 효과를 주는 제품이다. 또한 경미한 화상이나 피부 외상의 긴급 처치는 물론 습진 등의 피부질환에도 사용되는 등 전세계적으로 널리 사용되고 있다. Petrolatum (Vaseline) cosmetics are a personal care and cosmetic raw material that has a very significant effect such as moisture evaporation blocker, skin protection agent. In addition, it is widely used all over the world as it is used for urgent treatment of minor burns and skin trauma as well as skin diseases such as eczema.

그러나 수중유형 또는 유중수형의 제품에서 페트롤라툼 특유의 물성 때문에 사용이 불편하고 과량사용이 불가능하며, 과량 사용했다 하더라도 다른 원료와의 상용성 문제 및 안정성 문제로 인해 한계점이 분명하다. 이에 따라 페트롤라툼을 화장품제형에 적용시에는 크림 또는 소수의 로션타입 제형이나 밤타입 또는 연고 등 제약적으로 사용할 수 밖에 없다. 그래서 그 본래의 성능에 비해 다양한 제품군이 부족한 상황이다.However, in the oil-in-water or water-in-oil type products, the physical properties of petrolatum are inconvenient to use and cannot be used excessively, and even if used excessively, limitations are apparent due to compatibility problems with other raw materials and stability problems. Accordingly, when petrolatum is applied to cosmetic formulations, it is inevitably used as a cream or a small lotion type formulation or balm type or ointment. Thus, there is a lack of various product lines compared to the original performance.

선행기술문헌으로는, 대한민국 공개특허공보 10-2019-0012895에 천연 성분으로 구성된 고도로 개선된 물성을 가지는 페트롤라툼 젤리 대체제 및 이의 제조방법이, 대한민국 공개특허공보 10-2011-0138238에 안정하게 유지되면서 개선된 감촉을 위하여 10%를 초과하는 실리콘을 포함하는 페트롤라툼 기재 조성물이, 대한민국 공개특허공보 10-2018-0033179에 활성 성분들을 위한 페트롤라툼-계 전달 시스템이, 대한민국 공개특허공보 10-2018-0030543에 양이온성 살생물계를 포함하는 페트롤라툼-계 조성물이 각각 기재되어 있다. 그러나 상기 선행기술문헌에는 수용화가 가능한 페트롤라툼 조성물에 대한 기재나 이를 이용하여 별도의 분산, 용해 공정없이 안정된 화장료 조성물을 제조하는 방법에 대한 기재사항은 없다.In the prior art document, a petrolatum jelly substitute having a highly improved physical properties composed of natural ingredients in Korean Patent Publication No. 10-2019-0012895 and a method for preparing the same are maintained stably in Korean Patent Publication No. 10-2011-0138238 For petrolatum based compositions comprising more than 10% silicone for improved feel, petrolatum-based delivery systems for active ingredients are disclosed in Korean Patent Application Laid-Open No. 10-2018-0033179. 0030543 describes petrolatum-based compositions each comprising a cationic biocidal system. However, the prior art document does not have a description of a petrolatum composition that can be solubilized or a method of preparing a stable cosmetic composition without a separate dispersion and dissolution process using the same.

대한민국 공개특허공보 10-2019-0012895 (2019.02.11 공개)Republic of Korea Patent Publication 10-2019-0012895 (2019.02.11 published) 대한민국 공개특허공보 10-2011-0138238 (2011.12.26 공개)Republic of Korea Patent Publication No. 10-2011-0138238 (published Dec. 26, 2011) 대한민국 공개특허공보 10-2018-0033179 (2018.04.02 공개)Republic of Korea Patent Publication No. 10-2018-0033179 (published April 2, 2018) 대한민국 공개특허공보 10-2018-0030543 (2018.03.23 공개)Republic of Korea Patent Publication No. 10-2018-0030543 (2018.03.23 published)

본 발명은 수용화가 가능한 페트롤라툼 화장료 조성물의 제조방법에 관한 것이다.The present invention relates to a method for producing a petrolatum cosmetic composition capable of water solubility.

본 발명에 따르는 과제 해결수단은,The problem solving means according to the present invention,

페트롤라툼 조성물 20중량%, 정제수 67.7중량%, 부틸렌글라이콜 5중량%, 구아검 0.1중량%로 구성된 혼합물을 75℃까지 가열하고 균질기를 이용하여 2500RPM으로 5분간 교반시키는 제1단계;A first step of heating a mixture consisting of 20% by weight of petrolatum composition, 67.7% by weight of purified water, 5% by weight of butylene glycol, 0.1% by weight of guar gum to 75 ℃ and stirred at 2500 RPM for 5 minutes using a homogenizer;

상기 제1단계 결과물에 옥틸도데카놀 5중량%를 투입한 후, 유화시켜 균질기를 이용하여 2500RPM으로 5분간 교반시키는 제2단계;5 wt% of octyldodecanol was added to the resultant of the first step, followed by emulsification and stirring for 5 minutes at 2500 RPM using a homogenizer;

상기 제2단계 결과물에 소듐폴리아크릴레이트 0.2중량%를 투입시켜 균질기를 이용하여 3000RPM으로 5분간 교반시키는 제3단계; 및A third step of adding 0.2% by weight of sodium polyacrylate to the resultant of the second step and stirring the solution at 3000 RPM for 5 minutes using a homogenizer; And

상기 제3단계 결과물을 45~50℃까지 냉각 시킨 후 1,2-헥산다이올 2중량%를 투입하여 균질기를 이용하여 2500RPM으로 3분간 교반한 뒤, 30℃이하로 냉각하는 제4단계;를 포함하는 것을 특징으로 하는, 화장료 조성물의 제조방법이다.After cooling the resultant of the third step to 45 ~ 50 ℃ 2 wt% of 1,2-hexanediol was added and stirred for 3 minutes at 2500RPM using a homogenizer, the fourth step of cooling below 30 ℃; It is a manufacturing method of the cosmetic composition characterized by including.

상기에서, 페트롤라툼 조성물은,In the above, the petrolatum composition,

아이소펜틸다이올 20중량부, 세테아릴 알코올 15중량부 및 베헤닐 알코올15중량부를 65~80℃까지 가열하고 균질기(Homogenizer)를 이용하여 2000RPM으로 5분간 교반시키는 제1단계;A first step of heating 20 parts by weight of isopentyldiol, 15 parts by weight of cetearyl alcohol and 15 parts by weight of behenyl alcohol to 65-80 ° C., and stirring the same at 2000 RPM for 5 minutes using a homogenizer;

상기 제1단계의 결과물에 대두레시틴 10중량부를 투입한 후 용해하여 2000RPM으로 5분간 교반시키는 제2단계;A second step of adding 10 parts by weight of soybean lecithin to the resultant of the first step and dissolving the mixture for 5 minutes at 2000 RPM;

상기 제2단계의 결과물에 페트롤라툼 40중량부를 투입하여 균질기 3000RPM으로 5~20분간 교반시키는 제3단계; 및A third step of adding 40 parts by weight of petrolatum to the resultant of the second step and stirring the result with a homogenizer 3000RPM for 5 to 20 minutes; And

상기 제3단계의 결과물을 냉각시킨 다음 1200Bar의 압력으로 2회 내지 3회 고압균질기(Microfluidizer) 공정을 거치도록 하는 제4단계;를 포함하는 방법으로 제조된다.The fourth step of cooling the resultant of the third step and then subjected to a high-pressure homogenizer (Microfluidizer) 2 to 3 times at a pressure of 1200Bar; is prepared by a method comprising a.

본 발명에 따르는 과제 해결수단은,The problem solving means according to the present invention,

상기의 제조방법으로 제조된 화장료 조성물이다.It is a cosmetic composition prepared by the above production method.

상기의 조성물을 이용해 별도의 분산, 용해 공정없이 수화가 가능하며, 제한적으로 사용할 수밖에 없었던 페트롤라툼을 스킨, 에센스, 마스크팩 같은 여러 저점도 제형이나 기타 다양한 특이제형 개발이 가능하다.The composition can be hydrated without a separate dispersing and dissolving process, and various low viscosity formulations such as skin, essence, and mask pack or other specific formulations can be developed for petrolatum, which had to be limitedly used.

도 1A 및 도 1B는 실험예 1의 입자관찰 사진이다.
도 2는 실험예 2의 입자관찰 사진이다.
1A and 1B are particle observation photographs of Experimental Example 1. FIG.
2 is a particle observation photograph of Experimental Example 2.

이하에서는 본 발명의 이해를 돕기 위하여 실시예 등을 들어 상세히 설명하기로 한다. 그러나, 본 발명에 따른 실시예들은 여러 가지 다른 형태로 변형될 수 있으며, 본 발명의 범위가 하기 실시예들에 한정되는 것으로 해석되어서는 안 된다. 본 발명의 실시예들은 당업계에서 평균적인 지식을 가진자에게 본 발명을 보다 완전하게 설명하기 위해 제공되는 것이다. Hereinafter will be described in detail with reference to Examples and the like to help the understanding of the present invention. However, embodiments according to the present invention can be modified in many different forms, the scope of the invention should not be construed as limited to the following examples. Embodiments of the present invention are provided to more completely describe the present invention to those skilled in the art.

제조예 1. 수용화가 가능한 페트롤라툼 조성물 Preparation Example 1 Petrolatum Composition Acceptable

본 발명에 따른 수용화가 가능한 페트롤라툼 조성물은, 정제된 무색의 페트롤라툼, 블렌더로 사용되는 아이소펜틸다이올, 프로필렌글라이콜, 트리프로필렌글라이콜 및 펜틸렌글라이콜 중 하나 이상의 성분을 포함하는 폴리올류, 안정화제로 사용되는 주탄소수가 16개 이상 22개 이하인 고급알코올 및 유화제로 사용되는 대두레시틴을 포함한다.The water-soluble petrolatum composition according to the present invention comprises purified colorless petrolatum, at least one component of isopentyldiol, propylene glycol, tripropylene glycol and pentylene glycol used as a blender. Polyols, higher alcohols having 16 to 22 carbon atoms used as stabilizers and soybean lecithin used as emulsifiers.

바람직한 실시예로, 페트롤라툼 40중량부, 폴리올류 20중량부, 고급알코올 30중량부 및 대두레시틴 10중량부가 포함되도록 구성된다. 설계조건에 따라서, 상기 중량비율은 다소간 적절한 범위내에서 조절될 수 있다.In a preferred embodiment, 40 parts by weight of petrolatum, 20 parts by weight of polyols, 30 parts by weight of higher alcohol and 10 parts by weight of soy lecithin are included. Depending on the design conditions, the weight ratio may be adjusted to some extent within an appropriate range.

제조예 2. 수용화가 가능한 페트롤라툼 조성물의 제조방법Preparation Example 2 Method of Preparation of Petrolatum Composition Acceptable

제조예 1에 따른 페트롤라툼 조성물의 제조방법의 일예는 하기의 기재사항과 표 1과 같다.An example of the preparation method of petrolatum composition according to Preparation Example 1 is as described in Table 1 and the following.

아이소펜틸다이올 20중량부, 세테아릴 알코올 15중량부 및 베헤닐 알코올15중량부를 65~80℃까지 가열하고 균질기(Homogenizer)를 이용하여 2000RPM으로 5분간 교반시키는 제1단계;A first step of heating 20 parts by weight of isopentyldiol, 15 parts by weight of cetearyl alcohol and 15 parts by weight of behenyl alcohol to 65-80 ° C., and stirring the same at 2000 RPM for 5 minutes using a homogenizer;

상기 제1단계의 결과물에 대두레시틴 10중량부를 투입한 후 용해하여 2000RPM으로 5분간 교반시키는 제2단계;A second step of adding 10 parts by weight of soybean lecithin to the resultant of the first step and dissolving the mixture for 5 minutes at 2000 RPM;

상기 제2단계의 결과물에 페트롤라툼 40중량부를 투입하여 균질기 3000RPM으로 5~20분간 교반시키는 제3단계; 및A third step of adding 40 parts by weight of petrolatum to the resultant of the second step and stirring the result with a homogenizer 3000RPM for 5 to 20 minutes; And

상기 제3단계의 결과물을 냉각시킨 다음 1200Bar의 압력으로 2회 내지 3회 고압균질기(Microfluidizer) 공정을 거치도록 하는 제4단계;를 포함한다.And a fourth step of cooling the resultant of the third step and then performing a high pressure homogenizer (Microfluidizer) process two to three times at a pressure of 1200 Bar.

Prize INCI NameINCI Name 함량(%)content(%) 공정fair AA PolyolPolyol 2020 65~80℃ 가온 용해
균질기로 온도 유지하면서 교반 2000rpm, 5분
65 ~ 80 ℃ warm melting
Stirring while maintaining the temperature in a homogenizer 2000rpm, 5 minutes
Cetearyl AlcoholCetearyl alcohol 1515 Behenyl AlcoholBehenyl alcohol 1515 BB 대두레시틴Soybean Lecithin 1010 B상 투입 80℃ 가온 용해
균질기로 온도 유지하면서 교반 2000rpm, 5분
B phase input 80 ℃ heated melting
Stirring while maintaining the temperature in a homogenizer 2000rpm, 5 minutes
CC 페트롤라툼Petrolatum 4040 C상 투입 후 온도 유지하면서 균질기로 온도 유지하면서 교반 3000rpm, 20분 분산 확인After adding C phase, while maintaining the temperature with a homogenizer, keep stirring 3000rpm, dispersion for 20 minutes DD 고압균질화 단계High Pressure Homogenization Step -- 1200Bar 2회~3회 통과 후 종료Exit after passing 2 ~ 3 times of 1200Bar

제조예 3. 페트롤라툼 조성물을 적용한 화장료 조성물Preparation Example 3 Cosmetic Composition Applied Petrolatum Composition

제조예 1에 따르는 페트롤라툼 조성물을 적용한 화장물의 조성예는 다음과 같다.The composition of the cosmetics to which the petrolatum composition which concerns on manufacture example 1 is applied is as follows.

페트롤라툼 조성물; 및 부틸렌글라이콜, 구아검, 옥틸도데카놀, 소듐폴리아크릴레이트, 1,2-헥산다이올을 포함하는 기타조성물;을 포함하여 구성한다.Petrolatum compositions; And other compositions including butylene glycol, guar gum, octyldodecanol, sodium polyacrylate, and 1,2-hexanediol.

바람직하게는, 페트롤라툼 조성물 20중량부; 및 부틸렌글라이콜 5중량부, 구아검 0.1중량부, 옥틸도데카놀 5중량부, 소듐폴리아크릴레이트 0.2 중량부, 1,2-헥산다이올 2중량부를 포함하는 기타조성물;을 포함하여 구성한다.Preferably, 20 parts by weight of petrolatum composition; And other compositions including 5 parts by weight of butylene glycol, 0.1 parts by weight of guar gum, 5 parts by weight of octyldodecanol, 0.2 parts by weight of sodium polyacrylate, and 2 parts by weight of 1,2-hexanediol. do.

제조예 4. 페트롤라툼 조성물을 적용한 화장료 조성물의 제조방법Preparation Example 4 Manufacturing Method of Cosmetic Composition Applying Petrolatum Composition

제조예 3에 따르는 화장료 조성물의 제조방법의 일예는 다음과 같다. 설계조건에 따라, 하기 수치는 다소간 적절한 범위내에서 조절될 수 있다.An example of the manufacturing method of the cosmetic composition which concerns on manufacture example 3 is as follows. Depending on the design conditions, the following figures can be adjusted to some extent within an appropriate range.

페트롤라툼 조성물 20중량%, 정제수 67.7중량%, 부틸렌글라이콜 5중량%, 구아검 0.1중량%로 구성된 혼합물을 75℃까지 가열하고 균질기를 이용하여 2500RPM으로 5분간 교반시키는 제1단계;A first step of heating a mixture consisting of 20% by weight of petrolatum composition, 67.7% by weight of purified water, 5% by weight of butylene glycol, 0.1% by weight of guar gum to 75 ℃ and stirred at 2500 RPM for 5 minutes using a homogenizer;

상기 제1단계 결과물에 옥틸도데카놀 5중량%를 투입한 후, 유화시켜 균질기를 이용하여 2500RPM으로 5분간 교반시키는 제2단계;5 wt% of octyldodecanol was added to the resultant of the first step, followed by emulsification and stirring for 5 minutes at 2500 RPM using a homogenizer;

상기 제2단계 결과물에 소듐폴리아크릴레이트 0.2중량%를 투입시켜 균질기를 이용하여 3000RPM으로 5분간 교반시키는 제3단계; 및A third step of adding 0.2% by weight of sodium polyacrylate to the resultant of the second step and stirring the solution at 3000 RPM for 5 minutes using a homogenizer; And

상기 제3단계 결과물을 45~50℃까지 냉각 시킨 후 1,2-헥산다이올 2중량%를 투입하여 균질기를 이용하여 2500RPM으로 3분간 교반한 뒤, 30℃이하로 냉각하는 제4단계;를 포함한다.After cooling the resultant of the third step to 45 ~ 50 ℃ 2 wt% of 1,2-hexanediol was added and stirred for 3 minutes at 2500RPM using a homogenizer, the fourth step of cooling below 30 ℃; Include.

실험예 1. 제조예 1의 조성 및 제조예 2의 방법 검증Experimental Example 1. Composition of Preparation Example 1 and Method Verification of Preparation Example 2

[실험방법]Experimental Method

본 실험은 페트롤라툼 조성물의 최적 조성비와 고압균질기 공정의 수행여부를 검증하기 위하여 설계된 것이다.This experiment is designed to verify the optimal composition ratio of petrolatum composition and the performance of high pressure homogenizer process.

하기와 같이 표 2에 기재된 것과 같은 성분 및 함량으로 구성된 실시예의 페트롤라툼 조성물을 제조하였다.The petrolatum composition of the example consisting of the components and contents as described in Table 2 was prepared as follows.

A상을 80℃까지 가열하고 균질기(Homogenizer)를 이용하여 2000RPM으로 5분간 교반 후 B상을 A상에 투입한 후 용해하여 다시 5분간 같은 RPM으로 교반하였다. 다음 C상을 투입하여 균질기 3000RPM으로 20분간 교반한다. 냉각 후 고압균질기(Microfluidizer) 공정을 이용하여 1200Bar의 압력으로 최소 2회 최대 3회 통과하여 공정을 종료한다. Phase A was heated to 80 ° C., stirred for 5 minutes at 2000 RPM using a homogenizer, and then phase B was added to phase A, dissolved, and stirred at the same RPM for 5 minutes. Then add phase C and stir for 20 minutes with a homogenizer 3000RPM. After cooling, the microfluidizer process is used to terminate the process by passing a minimum of two times and a maximum of three times at a pressure of 1200Bar.

실시예 1~6에서는 고압균질기(Microfluidizer) 공정을 거친 실시예들이며, 비교예 1~6에서는 고압균질기(Microfluidizer) 공정을 거치지 않았다.In Examples 1 to 6 are examples that went through a high-pressure homogenizer (Microfluidizer) process, Comparative Examples 1 to 6 did not go through a high-pressure homogenizer (Microfluidizer) process.

상 (Phase)Phase 원료명Raw material name 실시예
1
Example
One
실시예
2
Example
2
실시예
3
Example
3
실시예
4
Example
4
실시예
5
Example
5
실시예
6
Example
6
함량(%)content(%) 함량(%)content(%) 함량(%)content(%) 함량(%)content(%) 함량(%)content(%) 함량(%)content(%) AA 아이소펜틸다이올Isopentyldiol 3030 2020 1010 2020 1010 -- 세테아릴알코올Cetearyl Alcohol 1515 1515 1515 2020 2020 2020 베헤닐알코올Behenyl Alcohol 1515 1515 1515 2020 2020 2020 BB 대두레시틴Soybean Lecithin 1010 1010 1010 1010 1010 1010 CC 페트롤라툼Petrolatum 3030 4040 5050 3030 4040 5050 상기 각 실시예 중 Microfluidizer 공정을 거치지 않은 것Each of the above examples did not undergo the Microfluidizer process 비교예
1
Comparative example
One
비교예
2
Comparative example
2
비교예
3
Comparative example
3
비교예
4
Comparative example
4
비교예
5
Comparative example
5
비교예
6
Comparative example
6

[성능평가][Performance evaluation]

표 3 및 도 1A, 도 1B과 같이 실시예 1~6, 비교예 1~6의 기본적인 성능평가를 위해 수용화도를 평가하고 입자사진 및 입자의 평균크기를 측정하였다.Table 3 and the water solubility was evaluated for the basic performance evaluation of Examples 1 to 6, Comparative Examples 1 to 6 as shown in Figure 1A, 1B, and measured the particle size and the average size of the particles.

수용화도 측정시 실시예 및 비교예의 조성물 20중량% 및 80℃의 정제수 80중량%를 Agi Mixer로 5분간 1500RPM으로 분산 뒤 30℃로 냉각하여 표면상태, 변색 및 부유물 유무를 육안으로 관찰하여 확인하였다. When measuring the water solubility, 20 wt% of the compositions of the Examples and Comparative Examples and 80 wt% of purified water at 80 ° C were dispersed at 1500 RPM for 5 minutes with Agi Mixer, and then cooled to 30 ° C to visually check the surface state, discoloration and the presence of suspended solids. .

입자관찰 및 입자측정시 Olympus社의 BX43을 이용하여 400배율 편광모드로 관찰 하였으며, 입자크기 측정은 Olympus社의 CellSens Entry 프로그램을 이용하여 측정하였다.Particle observation and particle measurement were performed using Olympus's BX43 in 400 magnification polarization mode, and particle size was measured using Olympus' CellSens Entry program.

실시예1Example 1 실시예 2Example 2 실시예 3Example 3 실시예 4Example 4 실시예 5Example 5 실시예 6Example 6 수용화도 측정Solubility Degree Measurement 가능possible 가능possible 불능Incapacity 가능possible 불능Incapacity 불능Incapacity 변색discoloration 안정stability 안정stability 변색discoloration 안정stability 변색discoloration 변색discoloration 부유물 존재여부Presence of floats 없음none 없음none 미약weak 없음none 미약weak 다수존재Majority 비교예1Comparative Example 1 비교예2Comparative Example 2 비교예3Comparative Example 3 비교예4Comparative Example 4 비교예5Comparative Example 5 비교예6Comparative Example 6 수용화도 측정Solubility Degree Measurement 가능possible 가능possible 불능Incapacity 가능possible 불능Incapacity 불능Incapacity 변색discoloration 미약weak 미약weak 변색discoloration 변색discoloration 변색discoloration 변색discoloration 부유물 존재여부Presence of floats 미약weak 미약weak 다수존재Majority 미약weak 다수존재Majority 다수존재Majority

결과를 검토하여 보면, 실시예 1, 2 및 4가 수용화도, 변색 및 부유물 평가에서 다른 실시예들보다 우수했음을 알 수 있다. 또한, 비교예 1, 2가 수용화도, 변색 및 부유물 평가에서 다른 실시예들보다 우수했음을 알 수 있다. In reviewing the results, it can be seen that Examples 1, 2 and 4 were superior to other examples in the degree of solubility, discoloration and suspension. In addition, it can be seen that Comparative Examples 1 and 2 were superior to other examples in the degree of water solubility, discoloration and suspension.

또한 실시예 1, 2는 비교예 1, 2보다 변색 및 부유물 평가에서 우수했음을 알 수 있다.In addition, it can be seen that Examples 1 and 2 were superior in discoloration and floating matter evaluation than Comparative Examples 1 and 2.

따라서 실시예 1 및 2의 조성 및 제조방법이 페트롤라툼의 수용화 및 원료 안정성면에서 우수할 것으로 예측된다고 하겠다. Therefore, the composition and preparation method of Examples 1 and 2 will be expected to be excellent in terms of water solubility and raw material stability of petrolatum.

실험예 2. 제조예 3의 조성 및 제조예 4의 방법 검증 Experimental Example 2. Composition of Preparation Example 3 and method verification of Preparation Example 4

[실험방법]Experimental Method

표 4를 살펴보면, 가장 성능이 좋을 것으로 예측되는 실시예 1, 2를 이용하여 제조된 수화 가능한 페르톨라툼 타입의 화장료 조성물 실시예 7, 8의 조성이 기재되어 있다. 그와 동시에 객관적인 비교 및 별도 유상부 혼합공정의 필요성 여부검증을 위해 실시예 1, 2에 함유된 성분함량을 별도로 각각 계량, 투입하여 비교예 7, 8을 제조하였다.Looking at Table 4, the compositions of Hydable Pertololaum Type Cosmetic Compositions Example 7, 8, prepared using Examples 1 and 2, which are expected to perform best, are described. At the same time, in order to objectively compare and verify whether the separate oil phase mixing process is necessary, the components of Examples 1 and 2 were separately weighed and added to prepare Comparative Examples 7, 8.

제조방법은 아래와 같다.The manufacturing method is as follows.

A상을 75℃까지 가열하고 균질기를 이용하여 2500RPM으로 5분간 교반 후 B상을 별도로 투입하여 80℃까지 가온, 용해시킨 후 A상에 투입하여 균질기를 이용하여 3000RPM으로 온도를 유지하며 5분간 교반한다. 유화가 잘 되었는지 확인 후 C상을 A상에 투입하여 온도를 유지하며 5분간 균질기를 이용하여 4000RPM으로 교반한다. 45~50℃까지 냉각 시킨 후 D상과 E상을 투입하여 균질기를 이용하여 2500RPM으로 3분간 교반 한 뒤, 30℃이하로 냉각하여 공정을 종료한다. Heat phase A to 75 ℃ and stir at 2500RPM for 5 minutes using homogenizer, then add phase B separately to warm up to 80 ℃, dissolve and add temperature to phase 3000 using A homogenizer to maintain temperature at 3000RPM and stir for 5 minutes. do. After confirming that the emulsification is good, the phase C is added to phase A to maintain the temperature, and then stirred at 4000 RPM using a homogenizer for 5 minutes. After cooling to 45 ~ 50 ℃ phase D and E phase was added and stirred for 3 minutes at 2500 RPM using a homogenizer, and then cooled to 30 ℃ or less to complete the process.

상 (Phase)Phase 원료명Raw material name 실시예7Example 7 실시예8Example 8 비교예7Comparative Example 7 비교예8Comparative Example 8 함량(%)content(%) 함량(%)content(%) 함량(%)content(%) 함량(%)content(%) AA 정제수Purified water To 100To 100 To 100To 100 To 100To 100 To 100To 100 부틸렌글라이콜Butylene Glycol 55 55 55 55 구아검Guar gum 0.10.1 0.10.1 0.10.1 0.10.1 이소펜틸다이올Isopentyldiol -- -- 44 44 실시예1Example 1 2020 -- -- -- 실시예2Example 2 -- 2020 -- -- BB 세테아릴알코올Cetearyl Alcohol -- -- 33 44 베헤닐알코올Behenyl Alcohol -- -- 33 44 대두레시틴Soybean Lecithin -- -- 22 22 페트롤라툼Petrolatum -- -- 88 66 옥틸도데카놀Octyldodecanol 55 55 55 55 CC 소듐폴리아크릴레이트Sodium Polyacrylate 0.200.20 0.200.20 0.200.20 0.200.20 DD 1,2-헥산다이올1,2-hexanediol 22 22 22 22

[성능평가][Performance evaluation]

표 4과 같이 제조한 유중수형 화장품을 평가하기 위해 표 5에 나와 있는 것과 같이 온도별 안정도 테스트 및 관능평가를 실시하였다.In order to evaluate the water-in-oil cosmetics prepared as shown in Table 4, the stability test and sensory evaluation for each temperature was performed as shown in Table 5.

또한 도 2와 같이 페트롤라툼이 유중수형 화장품내에서 합일현상 없이 안정하게 유지가 되는지에 대해 비교하기 위해 제조 30일 후의 입자를 측정하였다.Also, as shown in FIG. 2, particles were measured 30 days after preparation to compare whether petrolatum is stably maintained in the water-in-oil cosmetics without coalescence.

안정도Stability 관능평가Sensory evaluation -15℃-15 ℃ 4℃4 ℃ 25℃25 ℃ 37℃37 ℃ 50℃50 ℃ 사용감Feeling 보습력Moisturizing Odor 실시예 7Example 7 실시예 8Example 8 비교예 7Comparative Example 7 비교예 8Comparative Example 8

◎ : 양호 ○ : 보통 △ :미흡◎: Good ○: Normal △: Poor

상기와 같이 실시예 8이 원료안정도, 분산성 및 관능평가 등 여러 척도에서 현저히 개선된 성능을 나타냄을 알 수 있다.이는 실시예 2가 수용화도 및 안정성에서 매우 월등한 성능을 나타냄을 알 수 있다.As described above, it can be seen that Example 8 shows a remarkably improved performance in various measures such as raw material stability, dispersibility, and sensory evaluation. This shows that Example 2 shows very superior performance in water solubility and stability. .

다시말해, 제조예 1 및 제조예 2를 이용하여 제조된 실시예 2를 이용한 실시예 8이 매우 우수한 성능을 나타낸바, 제조예 1 내지 4의 조성 및 방법이 검증되었음을 알 수 있다.In other words, Example 8 using Example 2 prepared using Preparation Example 1 and Preparation Example 2 showed very good performance, and it can be seen that the compositions and methods of Preparation Examples 1 to 4 were verified.

이상의 설명은 본 발명의 기술 사상을 예시적으로 설명한 것에 불과한 것으로서, 본 발명이 속하는 기술 분야에서 통상의 지식을 가진 자라면 본 발명의 본질적인 특성에서 벗어나지 않는 범위에서 다양한 수정 및 변형이 가능할 것이다. The above description is merely illustrative of the technical idea of the present invention, and those skilled in the art to which the present invention pertains may make various modifications and changes without departing from the essential characteristics of the present invention.

따라서, 본 발명에 개시된 실시 예들은 본 발명의 기술 사상을 한정하기 위한 것이 아니라 설명하기 위한 것이고, 이러한 실시 예에 의하여 본 발명의 기술 사상의 범위가 한정되는 것은 아니다. 본 발명의 보호 범위는 아래의 청구범위에 의하여 해석되어야 하며, 그와 동등한 범위 내에 있는 모든 기술 사상은 본 발명의 권리범위에 포함되는 것으로 해석되어야 할 것이다.Therefore, the embodiments disclosed in the present invention are not intended to limit the technical idea of the present invention but to describe the present invention, and the scope of the technical idea of the present invention is not limited by these embodiments. The protection scope of the present invention should be interpreted by the following claims, and all technical ideas within the equivalent scope should be interpreted as being included in the scope of the present invention.

Claims (3)

유상부 혼합공정을 통해 제조되는 페트롤라툼 조성물 20중량%, 정제수 67.7중량%, 부틸렌글라이콜 5중량%, 구아검 0.1중량%로 구성된 혼합물을 75℃까지 가열하고 균질기를 이용하여 2500RPM으로 5분간 교반시키는 제1단계;
상기 제1단계 결과물에 옥틸도데카놀 5중량%를 투입한 후, 유화시켜 균질기를 이용하여 2500RPM으로 5분간 교반시키는 제2단계;
상기 제2단계 결과물에 소듐폴리아크릴레이트 0.2중량%를 투입시켜 균질기를 이용하여 3000RPM으로 5분간 교반시키는 제3단계; 및
상기 제3단계 결과물을 45~50℃까지 냉각 시킨 후 1,2-헥산다이올 2중량%를 투입하여 균질기를 이용하여 2500RPM으로 3분간 교반한 뒤, 30℃이하로 냉각하는 제4단계;를 포함하고,
상기 유상부 혼합공정은,
아이소펜틸다이올 20중량부, 세테아릴 알코올 15중량부 및 베헤닐 알코올15중량부를 65~80℃까지 가열하고 균질기(Homogenizer)를 이용하여 2000RPM으로 5분간 교반시키는 제1단계;
상기 제1단계의 결과물에 대두레시틴 10중량부를 투입한 후 용해하여 2000RPM으로 5분간 교반시키는 제2단계;
상기 제2단계의 결과물에 페트롤라툼 40중량부를 투입하여 균질기 3000RPM으로 5~20분간 교반시키는 제3단계; 및
상기 제3단계의 결과물을 냉각시킨 다음 1200Bar의 압력으로 2회 내지 3회 고압균질기(Microfluidizer) 공정을 거치도록 하는 제4단계;를 포함하는 방법으로 제조되는 것을 특징으로 하는, 화장료 조성물의 제조방법.
A mixture consisting of 20% by weight of petrolatum composition, 67.7% by weight of purified water, 5% by weight of butylene glycol, and 0.1% by weight of guar gum was heated to 75 ° C. and stirred at 2500 RPM for 5 minutes using a homogenizer. Making a first step;
5 wt% of octyldodecanol was added to the resultant of the first step, followed by emulsification and stirring for 5 minutes at 2500 RPM using a homogenizer;
A third step of adding 0.2% by weight of sodium polyacrylate to the resultant of the second step and stirring the solution at 3000 RPM for 5 minutes using a homogenizer; And
After cooling the resultant of the third step to 45 ~ 50 ℃ 2 wt% of 1,2-hexanediol was added and stirred for 3 minutes at 2500RPM using a homogenizer, the fourth step of cooling below 30 ℃; Including,
The oil phase mixing step,
A first step of heating 20 parts by weight of isopentyldiol, 15 parts by weight of cetearyl alcohol and 15 parts by weight of behenyl alcohol to 65-80 ° C., and stirring the same at 2000 RPM for 5 minutes using a homogenizer;
A second step of adding 10 parts by weight of soybean lecithin to the resultant of the first step and dissolving the mixture for 5 minutes at 2000 RPM;
A third step of adding 40 parts by weight of petrolatum to the resultant of the second step and stirring the result with a homogenizer 3000RPM for 5 to 20 minutes; And
The fourth step of cooling the resultant of the third step and then subjected to a high-pressure homogenizer (Microfluidizer) process 2 to 3 times at a pressure of 1200Bar; Production of a cosmetic composition, characterized in that it is prepared by a method comprising a Way.
삭제delete 청구항 1의 방법으로 제조된 화장료 조성물.
Cosmetic composition prepared by the method of claim 1.
KR1020190030786A 2019-03-18 2019-03-18 Manufacturing method of solubilized petrolatum cosmetic composition KR102026995B1 (en)

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JP2001072581A (en) * 1999-09-07 2001-03-21 Noevir Co Ltd Liquid emulsified composition for skin
JP4385170B2 (en) * 2007-07-20 2009-12-16 ロート製薬株式会社 Emulsified composition
KR20110138238A (en) 2009-04-15 2011-12-26 유니레버 엔.브이. Petrolatum based composition comprising greater than 10 % silicone for improved feel while remaining stable
KR101821934B1 (en) * 2017-10-12 2018-01-25 조상은 UV blocking compositions and process using the same
KR20180030543A (en) 2015-06-19 2018-03-23 글로벌 헬스 솔루션즈, 엘엘씨 Petrolatum-based compositions comprising cationic biocides
KR20190012895A (en) 2017-07-29 2019-02-11 주식회사 바이오스탠다드 An alternative for petrolatum jelly(vaselin) having highly improved properties consisting of only natural ingredients and a method for producing the same

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001072581A (en) * 1999-09-07 2001-03-21 Noevir Co Ltd Liquid emulsified composition for skin
JP4385170B2 (en) * 2007-07-20 2009-12-16 ロート製薬株式会社 Emulsified composition
KR20110138238A (en) 2009-04-15 2011-12-26 유니레버 엔.브이. Petrolatum based composition comprising greater than 10 % silicone for improved feel while remaining stable
KR20180030543A (en) 2015-06-19 2018-03-23 글로벌 헬스 솔루션즈, 엘엘씨 Petrolatum-based compositions comprising cationic biocides
KR20180033179A (en) 2015-06-19 2018-04-02 글로벌 헬스 솔루션즈, 엘엘씨 Petrolatum-system delivery system for active ingredients
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