KR101352405B1 - Manufacturing method of environmentally friendly polyester made from bio butanediol and nail care composition containing them - Google Patents

Manufacturing method of environmentally friendly polyester made from bio butanediol and nail care composition containing them Download PDF

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KR101352405B1
KR101352405B1 KR1020120012464A KR20120012464A KR101352405B1 KR 101352405 B1 KR101352405 B1 KR 101352405B1 KR 1020120012464 A KR1020120012464 A KR 1020120012464A KR 20120012464 A KR20120012464 A KR 20120012464A KR 101352405 B1 KR101352405 B1 KR 101352405B1
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environmentally friendly
friendly polyester
butanediol
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KR20130091154A (en
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오성기
한인선
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주식회사 케이씨아이
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/78Preparation processes
    • 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
    • A61K8/84Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/85Polyesters
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/02Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
    • C08G63/12Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L67/00Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
    • C08L67/02Polyesters derived from dicarboxylic acids and dihydroxy compounds

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Abstract

본 발명은 네일케어 조성물용 개질 폴리에스터의 제조방법 및 그 개질 폴리에스터가 함유된 네일케어 조성물에 관한 것으로, 더욱 상세하게는 2,3-부탄다이올과 아디프산을 반응기에 투입하는 혼합단계, 상기 혼합단계를 통해 혼합된 혼합물에 다관능성 단량체를 투입하는 단량체투입단계, 상기 다관능성 단량체가 투입된 혼합물을 가열하여 반응시키는 가열반응단계, 상기 가열반응단계를 거친 제조된 중합체를 냉각하는 냉각단계 및 상기 냉각단계를 거친 중합체에 용매를 투입하는 용매투입단계로 이루어진다.The present invention relates to a method for preparing a modified polyester for a nail care composition and a nail care composition containing the modified polyester, and more particularly, a mixing step of introducing 2,3-butanediol and adipic acid into a reactor. , A monomer input step of injecting a multifunctional monomer into the mixed mixture through the mixing step, a heating reaction step of heating and reacting the mixture into which the multifunctional monomer is added, and a cooling step of cooling the manufactured polymer after the heating reaction step And a solvent input step of introducing a solvent into the polymer that has undergone the cooling step.

Description

바이오 부탄다이올로부터 만들어진 친환경성 폴리에스터의 제조방법 및 그 친환경성 폴리에스터가 함유된 네일케어 조성물 {MANUFACTURING METHOD OF ENVIRONMENTALLY FRIENDLY POLYESTER MADE FROM BIO BUTANEDIOL AND NAIL CARE COMPOSITION CONTAINING THEM}MANUFACTURING METHOD OF ENVIRONMENTALLY FRIENDLY POLYESTER MADE FROM BIO BUTANEDIOL AND NAIL CARE COMPOSITION CONTAINING THEM}

본 발명은 친환경성 폴리에스터의 제조방법 및 그 친환경성 폴리에스터가 함유된 네일케어 조성물에 관한 것으로, 더욱 상세하게는 천연에서 얻은 당이나 글리세롤을 효소로 분해하여 제조된 2,3-부탄다이올이 사용되어 환경친화적인 친환경성 폴리에스터의 제조방법 및 그 친환경성 폴리에스터가 함유된 네일케이 조성물에 관한 것이다.
The present invention relates to a method for preparing an environmentally friendly polyester and a nail care composition containing the environmentally friendly polyester, and more particularly to 2,3-butanediol prepared by decomposing a sugar or glycerol obtained from a natural enzyme. The present invention relates to a method for producing an environmentally friendly eco-friendly polyester and a nail-k composition containing the eco-friendly polyester.

본 발명은 친환경성 폴리에스터의 제조방법 및 그 친환경성 폴리에스터가 함유된 네일케어 조성물에 관한 것으로, 더욱 상세하게는 천연에서 얻은 당이나 글리세롤을 효소로 분해하여 제조된 2,3-부탄다이올이 사용되어 환경친화적인 친환경성 폴리에스터의 제조방법 및 그 친환경성 폴리에스터가 함유된 네일케이 조성물에 관한 것이다.The present invention relates to a method for preparing an environmentally friendly polyester and a nail care composition containing the environmentally friendly polyester, and more particularly to 2,3-butanediol prepared by decomposing a sugar or glycerol obtained from a natural enzyme. The present invention relates to a method for producing an environmentally friendly eco-friendly polyester and a nail-k composition containing the eco-friendly polyester.

종래, 용제계 네일 케어 제품에는, 칠하기 쉬움, 윤기, 박리 특성 등의 여러가지 특성을 개량하기 위해서, 여러 가지의 합성수지가 배합되는데, 일본 특허 공개소 61-246113호 공보에는, 니트로셀룰로오스를 포함하는 네일 케어 제품 중에 베르사틱산글리시딜에스테르 변성 알키드 수지 등의 변성 알키드 수지와 슈크로오즈 벤조에이트를 병용하여 박리 특성 등을 개량한 네일 케어 제품가 개시되어 있다.Conventionally, various synthetic resins are compounded in solvent-based nail care products in order to improve various properties such as ease of painting, gloss, and peeling properties, but Japanese Patent Laid-Open No. 61-246113 includes nitrocellulose. A nail care product is disclosed in which a modified alkyd resin such as versatic acid glycidyl ester-modified alkyd resin and sucrose benzoate are used in combination in a nail care product to improve peeling properties.

또한, 일본 특허 공개평 5-213719호 공보에는, 상기 일본 특허 공개소 61-246113호 공보에 기재된 기술에 또한 실리콘계 그라프트 공중합체를 함유한, 박리 특성 등을 개량한 네일 케어 제품가 개시되어 있다.Further, Japanese Patent Laid-Open No. 5-213719 discloses a nail care product in which the peeling characteristics and the like, in which the technique described in Japanese Patent Laid-Open No. 61-246113 is further contained, contain a silicone-based graft copolymer, and the like.

이와 같이, 네일 케어 제품에 요구되는 여러 가지 특성의 향상을 도모한 제품의 연구, 개발이 성하게 행해지고 있다. 특히 최근, 소비자의 네일 케어 제품에 대한 보다 한층의 고품질화에 대한 요구가 높아져, 기호품의 다양화도 함께 많은 우수한 특성을 더불어 갖은 네일 케어 제품에 대한 요망이 종래보다 더 높아지고 있다.In this way, research and development of products aimed at improving various characteristics required for nail care products have been conducted. In particular, in recent years, the demand for higher quality of the nail care products for consumers is higher, and the demand for nail care products having many excellent characteristics along with the diversification of preferences is higher than before.

그러나 종래에 개발된 네일케어 제품에 사용되는 합성수지는 대부분 석유추출물로 이루어진 것이므로, 친환경적이지 못하고, 인체에 유해한 성분을 방출하는 문제점이 있었다.
However, since the synthetic resin used in the conventionally developed nail care products is mostly made of petroleum extract, it is not environmentally friendly, and there is a problem of releasing harmful ingredients to the human body.

본 발명의 목적은 천연에서 얻은 당이나 글리세롤을 효소로 분해하여 제조되는 2,3-부탄다이올을 이용하여 환경친화적인 친환경성 폴리에스터를 제조하는 방법 및 그 친환경성 폴리에스터가 함유된 네일케어 조성물을 제공하는 것이다.An object of the present invention is a method for producing an environmentally friendly eco-friendly polyester using 2,3-butanediol prepared by decomposing sugar or glycerol obtained from a natural enzyme and nail care containing the eco-friendly polyester It is to provide a composition.

본 발명의 다른 목적은 손톱에 바르기 쉽고, 손톱에 도포된 피막의 강도, 광택이 우수하며, 쉽게 박리되지 않는 네일케어 조성물을 제공하는 역할을 하는 친환경성 폴리에스터를 제조하는 방법 및 그 친환경성 폴리에스터가 함유된 네일케어 조성물을 제공하는 것이다.
Another object of the present invention is a method for producing an eco-friendly polyester which serves to provide a nail care composition that is easy to apply to nails, the strength and gloss of the coating applied to the nails, and is not easily peeled off and the eco-friendly poly It is to provide a nail care composition containing the ester.

본 발명의 목적은 2,3-부탄다이올과 아디프산을 반응기에 투입하는 혼합단계, 상기 혼합단계를 통해 혼합된 혼합물에 다관능성 단량체를 투입하는 단량체투입단계, 상기 다관능성 단량체가 투입된 혼합물을 가열하여 반응시키는 가열반응단계, 상기 가열반응단계를 거쳐 제조된 중합체를 냉각하는 냉각단계 및 상기 냉각단계를 거친 중합체에 용매를 투입하는 용매투입단계로 이루어지는 것을 특징으로 하는 친환경성 폴리에스터의 제조방법을 제공함에 의해 달성된다.An object of the present invention is a mixing step of injecting 2,3-butanediol and adipic acid into the reactor, a monomer input step of injecting a multifunctional monomer into the mixture mixed through the mixing step, a mixture in which the multifunctional monomer is added Preparation of eco-friendly polyester, characterized in that consisting of a heating reaction step of reacting by heating, a cooling step of cooling the polymer produced through the heating reaction step and a solvent input step of introducing a solvent into the polymer passed through the cooling step. By providing a method.

본 발명의 바람직한 특징에 따르면, 상기 2,3-부탄다이올은 당이나 글리세롤을 효소로 분해하여 제조되는 것으로 한다.According to a preferred feature of the present invention, the 2,3-butanediol is to be prepared by decomposing sugar or glycerol with an enzyme.

본 발명의 더 바람직한 특징에 따르면, 상기 혼합단계는 2,3-부탄다이올 100 중량부 및 아디프산 15 내지 25 중량부를 반응기에 투입하여 이루어지는 것으로 한다.According to a more preferred feature of the invention, the mixing step is to be made by adding 100 parts by weight of 2,3-butanediol and 15 to 25 parts by weight of adipic acid into the reactor.

본 발명의 더욱 바람직한 특징에 따르면, 상기 단량체투입단계는 상기 혼합단계를 통해 혼합된 혼합물 100 중량부에 다관능성 단량체인 무수트리멜리트 33 내지 37 중량부를 투입하여 이루어지는 것으로 한다.According to a more preferred feature of the invention, the monomer input step is to be made by adding 33 to 37 parts by weight of an anhydrous trimellitic as a multifunctional monomer to 100 parts by weight of the mixture mixed through the mixing step.

본 발명의 더욱 더 바람직한 특징에 따르면, 상기 가열반응단계는 상기 다관능성 단량체가 투입된 혼합물을 170 내지 190℃의 온도로 가열하여 반응시키는 것으로 한다.According to a further preferred feature of the present invention, the heating reaction step is to react by heating the mixture into which the multifunctional monomer is added to a temperature of 170 to 190 ℃.

본 발명의 더욱 더 바람직한 특징에 따르면, 상기 냉각단계는 상기 가열반응단계를 거쳐 제조된 중합체를 120 내지 130℃의 온도로 냉각하는 것으로 한다.According to a further preferred feature of the invention, the cooling step is to cool the polymer produced through the heating reaction step to a temperature of 120 to 130 ℃.

본 발명의 더욱 더 바람직한 특징에 따르면, 상기 용매투입단계는 상기 냉각단계를 거친 중합체 100 중량부에 용매 30 내지 40 중량부를 투입하여 이루어지는 것으로 한다.According to a further preferred feature of the invention, the solvent input step is to be made by adding 30 to 40 parts by weight of the solvent to 100 parts by weight of the polymer after the cooling step.

본 발명의 더욱 더 바람직한 특징에 따르면, 상기 용매는 부틸아세테이트인 것으로 한다.
According to a still further preferred feature of the present invention, the solvent is assumed to be butyl acetate.

또한, 본 발명의 목적은 상기 친환경성 폴리에스터의 제조방법을 통해 제조된 친환경성 폴리에스터가 함유되는 것을 특징으로 하는 네일케어 조성물을 제공함에 의해서도 달성될 수 있다.
In addition, an object of the present invention can be achieved by providing a nail care composition, characterized in that it contains an environmentally friendly polyester produced through the manufacturing method of the environmentally friendly polyester.

본 발명에 따른 친환경성 폴리에스터의 제조방법 및 그 친환경성 폴리에스터가 함유된 네일케어 조성물은 천연에서 얻은 당이나 글리세롤을 효소로 분해하여 제조되는 2,3-부탄다이올이 사용되어 환경친화적인 친환경성 폴리에스터 및 그 친환경성 폴리에스터가 함유된 네일케어 조성물을 제공하는 탁월한 효과를 나타낸다.Eco-friendly polyester manufacturing method and nail care composition containing the eco-friendly polyester according to the present invention is environmentally friendly by using 2,3-butanediol prepared by decomposing sugar or glycerol obtained from the natural enzyme It shows an excellent effect of providing an eco-friendly polyester and a nail care composition containing the eco-friendly polyester.

또한, 손톱에 바르기 쉽고, 손톱에 도포된 피막의 강도, 광택이 우수하며, 쉽게 박리되지 않는 네일케어 조성물을 제공하는 역할을 하는 친환경성 폴리에스터 및 그 개질폴리에스터가 함유된 네일케어 조성물을 제공하는 탁월한 효과를 나타낸다.
In addition, it provides a nail care composition containing an environmentally-friendly polyester and its modified polyester, which is easy to apply to the nail, excellent strength, luster of the film applied to the nail, and serves to provide a nail care composition that does not easily peel off Excellent effect.

도 1은 본 발명에 따른 친환경성 폴리에스터의 제조방법을 나타낸 순서도이다.
도 2는 본 발명의 실시예 1을 통해 제조된 친환경성 폴리에스터를 FT-IR로 분석하여 나타낸 그래프이다.
도 3은 본 발명의 비교예 4를 통해 제조된 폴리에스터를 FT-IR로 분석하여 나타낸 그래프이다.
1 is a flow chart showing a method for producing an environmentally friendly polyester according to the present invention.
Figure 2 is a graph showing the analysis of the eco-friendly polyester produced in Example 1 of the present invention by FT-IR.
Figure 3 is a graph showing the analysis of the polyester produced by Comparative Example 4 of the present invention by FT-IR.

이하에는, 본 발명의 바람직한 실시예와 각 성분의 물성을 상세하게 설명하되, 이는 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자가 발명을 용이하게 실시할 수 있을 정도로 상세하게 설명하기 위한 것이지, 이로 인해 본 발명의 기술적인 사상 및 범주가 한정되는 것을 의미하지는 않는다.
Hereinafter, preferred embodiments of the present invention and physical properties of the respective components will be described in detail with reference to the accompanying drawings. However, the present invention is not limited thereto, And this does not mean that the technical idea and scope of the present invention are limited.

본 발명에 따른 친환경성 폴리에스터의 제조방법은 2,3-부탄다이올과 아디프산을 반응기에 투입하는 혼합단계(S101), 상기 혼합단계(S101)를 통해 혼합된 혼합물에 다관능성 단량체를 투입하는 단량체투입단계(S103), 상기 다관능성 단량체가 투입된 혼합물을 가열하여 반응시키는 가열반응단계(S105), 상기 가열반응단계(S105)를 거쳐 제조된 중합체를 냉각하는 냉각단계(S107) 및 상기 냉각단계(S107)를 거친 중합체에 용매를 투입하는 용매투입단계(S109)로 이루어진다.
Method for producing an environmentally friendly polyester according to the present invention is a mixing step (S101) to add 2,3-butanediol and adipic acid to the reactor, the multifunctional monomer in the mixture through the mixing step (S101) The monomer input step (S103) to be injected, the heating reaction step (S105) for heating and reacting the mixture into which the multifunctional monomer is added, the cooling step (S107) for cooling the polymer produced through the heating reaction step (S105) and the It is made of a solvent input step (S109) for introducing a solvent to the polymer passed through the cooling step (S107).

상기 혼합단계(S101)는 2,3-부탄다이올과 아디프산을 반응기에 투입하는 단계로, 2,3-부탄다이올 100 중량부 및 아디프산 15 내지 25 중량부를 교반장치 및 탈수용 콘덴서 등이 구비된 반응기에 투입하여 이루어지는데, 이때, 상기 2,3-부탄다이올은 천연에서 얻은 당이나 글리세롤을 효소인 리파아제(lipase)로 분해하여 제조된다.The mixing step (S101) is a step of adding 2,3-butanediol and adipic acid to the reactor, 100 parts by weight of 2,3-butanediol and 15 to 25 parts by weight of adipic acid for stirring and dehydration The 2,3-butanediol is prepared by decomposing a sugar or glycerol obtained from a natural substance into a lipase which is an enzyme.

이러한 혼합단계(S101)에서 투입된 2,3-부탄다이올과 아디프산은 상기 가열반응단계(S105)에서 중합반응을 진행하여 중합체로 제조되며, 이러한 반응을 통해 제조되는 폴리에스터는 천연에서 얻은 당이나 글리세롤로부터 분해된 2,3-부탄다이올이 사용되어 친환경적인 효과를 나타낸다.2,3-butanediol and adipic acid introduced in the mixing step (S101) are produced as a polymer by the polymerization reaction in the heating reaction step (S105), the polyester produced through this reaction is a sugar obtained from nature 2,3-butanediol decomposed from or glycerol is used to exhibit an environmentally friendly effect.

이러한 2,3-부탄다이올과 아디프산의 중합반응을 통해 폴리에스터가 제조되는 반응식을 아래에 나타내었다.The reaction scheme for preparing the polyester through the polymerization of 2,3-butanediol and adipic acid is shown below.

Figure 112012010010717-pat00001
Figure 112012010010717-pat00001

Figure 112012010010717-pat00002

Figure 112012010010717-pat00002

상기 단량체투입단계(S103)는 상기 혼합단계(S101)를 통해 혼합된 혼합물에 다관능성 단량체를 투입하는 단계로, 상기 혼합단계(S101)를 통해 혼합된 혼합물 100 중량부에 다관능성 단량체인 무수트리멜리트(trimellitic anhydride) 33 내지 37 중량부를 투입하여 이루어지는데, 상기 무수트리멜리트가 투입되면, 점도가 증가되어 손톱에 바르기 쉽고, 손톱에 도포된 피막의 강도, 광택이 우수하며, 쉽게 박리되지 않는 효과를 나타내는 폴리에스터가 제조된다.The monomer input step (S103) is a step of injecting a multifunctional monomer into the mixture mixed through the mixing step (S101), anhydrous tree which is a multifunctional monomer in 100 parts by weight of the mixed mixture through the mixing step (S101) It is made by adding 33 to 37 parts by weight of trimellitic anhydride, and when the anhydrous trimellit is added, the viscosity is increased, so that it is easy to be applied to the nail, the strength and gloss of the film applied to the nail is excellent, and not easily peeled off. A polyester is produced that does not have an effect.

상기 무수트리멜리트 33 내지 37 중량부는 상기 혼합물에 3회에 나눠서 투입하며, 상기 반응기에 구비된 교반장치를 이용하여 상기 무수트리멜리트가 상기 혼합물에 완전하게 용해될 때까지 교반을 진행하는 것이 바람직하다.
33 to 37 parts by weight of the anhydrous trimellit is added to the mixture in three portions, and the stirring is performed until the anhydrous trimellit is completely dissolved in the mixture using a stirring device provided in the reactor. desirable.

상기 가열반응단계(S105)는 상기 다관능성 단량체가 투입된 혼합물을 가열하여 반응시키는 단계로, 상기 다관능성 단량체가 투입된 혼합물을 170 내지 190℃의 온도로 가열하여 중합반응이 진행되도록 하는데, 이때, 혼합물은 8 내지 10/hr으로 서서히 승온시키며, 중합반응 과정에서 생성되는 물은 상기 반응기에 구비된 탈수용 콘데서를 이용하여 제거하면서 중합반응을 진행해야 중합효율과 중합시간이 단축된다.
The heating reaction step (S105) is a step of heating and reacting the mixture into which the multifunctional monomer is added, and heating the mixture to which the polyfunctional monomer is added to a temperature of 170 to 190 ° C., whereby the polymerization reaction proceeds. The temperature is gradually increased to 8 to 10 / hr, and the water generated in the polymerization process is removed by using a dehydration condenser provided in the reactor to proceed with the polymerization reaction to shorten the polymerization efficiency and polymerization time.

상기 냉각단계(S107)는 상기 가열반응단계(S105)를 거쳐 제조된 중합체를 냉각하는 단계로, 상기 가열반응단계(S105)를 거쳐 제조된 중합체를 120 내지 130℃의 온도로 냉각하여 중합반응을 중단시키고 안정화하는 단계다.The cooling step (S107) is a step of cooling the polymer produced through the heating reaction step (S105), by cooling the polymer prepared through the heating reaction step (S105) to a temperature of 120 to 130 ℃ to polymerization reaction It is the stage of stopping and stabilizing.

이때, 상기 냉각단계(S107)를 진행하기 전에는 상기 가열반응단계(S105)에서 중합반응을 통해 중합된 중합체의 산가를 측정하여 중합체의 산가가 45 내지 55의 범위로 측정되면 냉각단계(S107)를 진행하는 것이 바람직하다.
At this time, before proceeding with the cooling step (S107), if the acid value of the polymer is measured in the range of 45 to 55 by measuring the acid value of the polymer polymerized by the polymerization reaction in the heating reaction step (S105) the cooling step (S107) It is preferable to proceed.

상기 용매투입단계(S109)는 상기 냉각단계(S107)를 거친 중합체에 용매를 투입하는 단계로, 상기 냉각단계(S107)를 거친 중합체 100 중량부에 용매 30 내지 40 중량부를 투입하여 이루어지는데, 반응기에 질소가스를 200 내지 300ml/min의 속도로 주입하면서 이루어지는 것이 바람직하다.The solvent input step (S109) is a step of adding a solvent to the polymer passed through the cooling step (S107), made by adding 30 to 40 parts by weight of the solvent to 100 parts by weight of the polymer passed through the cooling step (S107), the reactor It is preferable that the gas is injected into the nitrogen gas at a rate of 200 to 300 ml / min.

이때, 상기 용매는 부틸아세테이트로 이루어지며, 상기 중합체의 점도를 조절하는 역할을 한다.
At this time, the solvent is made of butyl acetate, and serves to adjust the viscosity of the polymer.

또한, 본 발명에 따른 네일케어 조성물은 상기 친환경성 폴리에스터의 제조방법을 통해 제조된 친환경성 폴리에스터가 함유되어 이루어진다.In addition, the nail care composition according to the present invention comprises an environmentally friendly polyester produced through the manufacturing method of the environmentally friendly polyester.

상기 네일케어 조성물은 네일케어용 조성물 50 내지 70 중량부에 상기 친환경성 폴리에스터의 제조방법을 통해 제조된 친환경성 폴리에스터가 30 내지 50 중량부 함유되는데, 이때, 상기 네일케어용 조성물은 네일케어 조성물에 사용되는 성분이면 어떠한 것이든 사용가능하며, 특별히 한정되지 않지만, 용매, 침전방지제, 분산제, 도막형성요소(Film former), 가소제 및 자외선 차단제 등으로 이루어지는 것이 바람직하다.The nail care composition contains 30 to 50 parts by weight of environmentally friendly polyester prepared by the method for producing an environmentally friendly polyester in 50 to 70 parts by weight of the nail care composition, wherein the nail care composition is nail care Any component can be used as long as it is a component used in the composition, and is not particularly limited, but is preferably composed of a solvent, a precipitation inhibitor, a dispersant, a film former, a plasticizer, a sunscreen, and the like.

더욱 바람직하게는, 상기 용매는 에틸아세테이트 또는 부틸아세테이트로 이루어지며, 상기 침전방지제는 벤토나이트(bentonite), 인산으로 이루어지고, 상기 분산제는 무수에탄올(Anhydrous Ethanol)로 이루어지며, 상기 도막형성요소는 1/2 또는 1/4 의 니트로셀룰로오스로 이루어지고, 상기 가소제는 아세틸트리부틸시트레이트, 에틸셀루솔브(Ethyl Cellosolve), 캠퍼(Camphor)로 이루어진다.More preferably, the solvent is ethyl acetate or butyl acetate, the precipitation inhibitor is made of bentonite, phosphoric acid, the dispersing agent is made of anhydrous Ethanol, the coating film forming element is 1 / 2 or 1/4 nitrocellulose, the plasticizer is acetyltributyl citrate, ethyl cellosolve (Ethyl Cellosolve), Camper (Camphor).

이러한 성분으로 이루어진 네일케어 조성물은 네일케어용 조성물이 갖는 고유의 물성뿐만 아니라, 친환경성 폴리에스터의 제조방법을 통해 제조된 친환경성 폴리에스터가 함유되어 친환경적이며, 상기 친환경성 폴리에스터가 갖는 우수한 점성, 접착성 및 광택성으로 인해 손톱에 바르기 쉽고, 손톱에 도포된 피막의 강도, 광택이 우수하며, 쉽게 박리되지 않는 효과를 나타낸다.
Nail care composition consisting of these ingredients is not only inherent in the physical properties of the composition for nail care, but also contains eco-friendly polyester produced through the manufacturing method of eco-friendly polyester is eco-friendly, excellent viscosity of the eco-friendly polyester Because of the adhesiveness and glossiness, it is easy to apply to the nail, and the film applied to the nail is excellent in strength and luster, and does not easily peel off.

이하에서는, 본 발명에 따른 친환경성 폴리에스터의 제조방법 및 그 제조방법을 통해 제조된 친환경성 폴리에스터의 물성을 실시예를 들어 설명한다.
Hereinafter, the physical properties of the eco-friendly polyester produced by the method and the manufacturing method of the eco-friendly polyester according to the present invention will be described with an example.

<실시예 1>&Lt; Example 1 >

2,3-부탄다이올 100 중량부에 아디프산 20 중량부를 교반장치 및 탈수용 콘덴서가 구비된 반응기에 투입하여 혼합물을 제조하고, 상기 혼합물 100 중량부에 무수트리멜리트 33 중량부를 투입하고, 상기 무수트리멜리트 33 중량부가 투입된 혼합물을 170℃의 온도로 가열하고 중합반응을 진행하여 중합체를 제조하고, 상기 중합체의 산가를 측정한 후에 130℃의 온도로 냉각하고, 상기의 온도로 냉각된 중합체 100 중량부에 부틸아세테이트 35 중량부를 투입하여 친환경성 폴리에스터를 제조하였다.
20 parts by weight of adipic acid was added to 100 parts by weight of 2,3-butanediol in a reactor equipped with a stirring device and a dehydrating condenser to prepare a mixture, and 33 parts by weight of anhydrous trimellit was added to 100 parts by weight of the mixture. After heating the mixture to which 33 parts by weight of the anhydrous trimellit was added at a temperature of 170 ° C., a polymerization reaction was performed to prepare a polymer, the acid value of the polymer was measured, and then cooled to a temperature of 130 ° C., and cooled to the temperature described above. 35 parts by weight of butyl acetate was added to 100 parts by weight of the polymer to prepare an eco-friendly polyester.

<실시예 2><Example 2>

상기 실시예 1과 동일하게 진행하되, 180℃ 온도에서 중합반응을 진행하여 친환경성 폴리에스터를 제조하였다.
Proceed in the same manner as in Example 1, to proceed with the polymerization at 180 ℃ to prepare an environmentally friendly polyester.

<실시예 3><Example 3>

상기 실시예 1과 동일하게 진행하되, 190℃의 온도에서 중합반응을 진행하여 친환경성 폴리에스터를 제조하였다.
Proceed in the same manner as in Example 1, proceeding the polymerization at a temperature of 190 ℃ to prepare an environmentally friendly polyester.

<비교예 1>&Lt; Comparative Example 1 &

상기 실시예 1과 동일하게 진행하되, 160℃의 온도에서 중합반응을 진행하였다.
In the same manner as in Example 1, the polymerization was carried out at a temperature of 160 ℃.

상기 실시예 1 내지 3을 통해 진행된 중합반응 시간 및 중합반응을 통해 제조된 중합체의 산가를 측정하여 아래 표 1에 나타내었다.
The polymerization time proceeded through Examples 1 to 3 and the acid value of the polymer produced through the polymerization reaction was measured and shown in Table 1 below.

<표 1>TABLE 1

Figure 112012010010717-pat00003
Figure 112012010010717-pat00003

위에 표 1에 나타낸 것처럼 중합반응은 170℃의 온도에서 진행되는 것을 알 수 있다.As shown in Table 1 above, it can be seen that the polymerization proceeds at a temperature of 170 ° C.

또한, 중합반응의 온도가 상승하면, 반응완료 시간은 짧아지고, 산가는 낮아지는 것을 알 수 있다.
In addition, when the temperature of a polymerization reaction rises, it turns out that reaction completion time becomes short and an acid value becomes low.

<실시예 4><Example 4>

상기 실시예 1과 동일하게 진행하되, 175℃의 온도에서 중합반응을 진행하여 친환경성 폴리에스터를 제조하였다.
Proceed in the same manner as in Example 1, proceeding the polymerization at a temperature of 175 ℃ to prepare an environmentally friendly polyester.

<실시예 5><Example 5>

상기 실시예 1과 동일하게 진행하되, 무수트리멜리트 35 중량부를 투입하고, 175℃의 온도에서 중합반응을 진행하여 친환경성 폴리에스터를 제조하였다.
Proceed in the same manner as in Example 1, 35 parts by weight of anhydrous trimellit was added, and a polymerization reaction was performed at a temperature of 175 ° C. to produce an eco-friendly polyester.

<실시예 6><Example 6>

상기 실시예 1과 동일하게 진행하되, 무수트리멜리트 37 중량부를 투입하고, 175℃의 온도에서 중합반응을 진행하여 친환경성 폴리에스터를 제조하였다.
Proceed in the same manner as in Example 1, 37 parts by weight of anhydrous trimellit was added, and an environmentally friendly polyester was prepared by performing a polymerization reaction at a temperature of 175 ° C.

<비교예 2>Comparative Example 2

상기 실시에 1과 동일하게 진행하되, 무수트리멜리트 40 중량부를 투입하고, 175℃의 온도에서 중합반응을 진행하여 친환경성 폴리에스터를 제조하였다.
Proceed in the same manner as in Example 1, 40 parts by weight of anhydrous trimellit was added, and a polymerization reaction was performed at a temperature of 175 ° C. to produce an environmentally friendly polyester.

상기 실시예 4 내지 6 및 비교예 2를 통해 제조된 친환경성 폴리에스터의 산가 및 점도를 측정하여 아래 표 2에 나타내었다.
The acid value and viscosity of the eco-friendly polyester prepared through Examples 4 to 6 and Comparative Example 2 were measured and shown in Table 2 below.

<표 2><Table 2>

Figure 112012010010717-pat00004
Figure 112012010010717-pat00004

위에 표 2에 나타낸 것처럼 무수트리멜리트의 함량이 증가하면 점도가 증가하는 것을 알 수 있다.
As shown in Table 2 above, it can be seen that the viscosity increases when the content of the anhydrous trimellit is increased.

<실시예 7>&Lt; Example 7 >

상기 실시예 1과 동일하게 진행하되, 2,3-부탄다이올 100 중량부에 아디프산 17.5 중량부를 투입하여 친환경성 폴리에스터를 제조하였다.
Proceed in the same manner as in Example 1, 17.5 parts by weight of adipic acid was added to 100 parts by weight of 2,3-butanediol to prepare an eco-friendly polyester.

<실시예 8>&Lt; Example 8 >

상기 실시예 1과 동일하게 진행하되, 2,3-부탄다이올 100 중량부에 아디프산 15 중량부를 투입하여 친환경성 폴리에스터를 제조하였다.
Proceed in the same manner as in Example 1, by adding 15 parts by weight of adipic acid to 100 parts by weight of 2,3-butanediol to prepare an environmentally friendly polyester.

<비교예 3>&Lt; Comparative Example 3 &

상기 실시예 1과 동일하게 진행하되, 2,3-부탄다이올 100 중량부에 아디프산 11 중량부를 투입하여 친환경성 폴리에스터를 제조하였다.
Proceed in the same manner as in Example 1, by adding 11 parts by weight of adipic acid to 100 parts by weight of 2,3-butanediol to prepare an environmentally friendly polyester.

상기 실시예 7 내지 8 및 비교예 1을 통해 제조된 친환경성 폴리에스터의 산가 및 점도를 측정하여 아래 표 3에 나타내었다.
The acid value and viscosity of the eco-friendly polyester prepared through Examples 7 to 8 and Comparative Example 1 were measured and shown in Table 3 below.

<표 3><Table 3>

Figure 112012010010717-pat00005
Figure 112012010010717-pat00005

위에 표 3에 나타낸 것처럼 아디프산의 함량비율이 줄어들면 점도가 감소하는 것을 알 수 있다.
As shown in Table 3 above, it can be seen that the viscosity decreases when the content ratio of adipic acid decreases.

<비교예 4>&Lt; Comparative Example 4 &

실시예 1과 동일하게 진행하되, 2,3-부탄다이올 대신 네오펜틸글리콜을 사용하여 폴리에스터를 제조하였다.
Proceed in the same manner as in Example 1, using neopentyl glycol instead of 2,3-butanediol to prepare a polyester.

상기 실시예 1과 비교예 4를 통해 제조된 친환경성 폴리에스터 및 폴리에스터를 FT-IR 분석하여 도 2 및 3에 나타내었다.Environmentally friendly polyesters and polyesters prepared through Example 1 and Comparative Example 4 are shown in FIGS. 2 and 3 by FT-IR analysis.

도 2 내지 3에 나타낸 것처럼, 본 발명에 의해 제조된 친환경성 폴리에스터는 비교예 4를 통해 제조된 폴리에스터와 유사한 물성을 나타내면서도 환경친화적인 효과를 나타낸다.
As shown in Figures 2 to 3, the eco-friendly polyester produced by the present invention shows similar properties to the polyester produced through Comparative Example 4, but also shows an environmentally friendly effect.

S101 ; 혼합단계
S103 ; 단량체투입단계
S105 ; 가열반응단계
S107 ; 냉각단계
S109 ; 용매투입단계
S101; Mixing step
S103; Monomer input step
S105; Heating reaction stage
S107; Cooling step
S109; Solvent input step

Claims (9)

천연 글리세롤을 효소로 분해하여 제조된 2,3-부탄다이올 100중량부와 아디프산 15내지 25중량부를 반응기에 투입하는 혼합단계;
상기 혼합단계를 통해 혼합된 혼합물 100중량부에 다관능성 단량체인 무수트리멜리트 33 내지 37중량부를 투입하는 단량체투입단계;
상기 다관능성 단량체가 투입된 혼합물을 가열하여 반응시키는 가열반응단계;
상기 가열반응단계를 거쳐 제조된 중합체를 냉각하는 냉각단계; 및
상기 냉각단계를 거친 중합체에 용매를 투입하는 용매투입단계;로 이루어지는 것을 특징으로 하는 친환경성 폴리에스터의 제조방법.
A mixing step of introducing 100 parts by weight of 2,3-butanediol and 15 to 25 parts by weight of adipic acid prepared by decomposing the natural glycerol into an reactor;
A monomer input step of adding 33 to 37 parts by weight of anhydrous trimellitate as a multifunctional monomer to 100 parts by weight of the mixture mixed through the mixing step;
A heating reaction step of heating and reacting the mixture into which the multifunctional monomer is added;
A cooling step of cooling the polymer prepared through the heating reaction step; And
Method of producing an environmentally friendly polyester, characterized in that consisting of; a solvent input step of injecting a solvent into the polymer after the cooling step.
삭제delete 삭제delete 삭제delete 청구항 1에 있어서,
상기 가열반응단계는 상기 다관능성 단량체가 투입된 혼합물을 170 내지 190℃의 온도로 가열하여 반응시키는 것을 특징으로 하는 친환경성 폴리에스터의 제조방법.
The method according to claim 1,
The heating reaction step is a method for producing an environmentally friendly polyester, characterized in that for reacting by heating the mixture into which the multifunctional monomer is added at a temperature of 170 to 190 ℃.
청구항 1에 있어서,
상기 냉각단계는 상기 가열반응단계를 거쳐 제조된 중합체를 120 내지 130℃의 온도로 냉각하는 것을 특징으로 하는 친환경성 폴리에스터의 제조방법.
The method according to claim 1,
The cooling step is a method for producing an eco-friendly polyester, characterized in that for cooling the polymer produced through the heating reaction step to a temperature of 120 to 130 ℃.
청구항 1에 있어서,
상기 용매투입단계는 상기 냉각단계를 거친 중합체 100 중량부에 용매 30 내지 40 중량부를 투입하여 이루어지는 것을 특징으로 하는 친환경성 폴리에스터의 제조방법.
The method according to claim 1,
The solvent input step is a method for producing an environmentally friendly polyester, characterized in that by adding 30 to 40 parts by weight of the solvent to 100 parts by weight of the polymer after the cooling step.
청구항 1에 있어서,
상기 용매는 부틸아세테이트인 것을 특징으로 하는 친환경성 폴리에스터의 제조방법.
The method according to claim 1,
The solvent is a method for producing environmentally friendly polyester, characterized in that butyl acetate.
삭제delete
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4600768A (en) 1985-10-18 1986-07-15 Eastman Kodak Company Aromatic polyesters derived from 2,3-butanediol
KR100200415B1 (en) 1996-07-26 1999-06-15 한형수 Process for preparing biodegradable aliphatic copolyester
JP2010037463A (en) 2008-08-06 2010-02-18 Nitto Denko Corp Polyester, polyester composition, adhesive composition, adhesive layer, and adhesive sheet

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4600768A (en) 1985-10-18 1986-07-15 Eastman Kodak Company Aromatic polyesters derived from 2,3-butanediol
KR100200415B1 (en) 1996-07-26 1999-06-15 한형수 Process for preparing biodegradable aliphatic copolyester
JP2010037463A (en) 2008-08-06 2010-02-18 Nitto Denko Corp Polyester, polyester composition, adhesive composition, adhesive layer, and adhesive sheet

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