JP4553607B2 - Oil-in-water emulsified fragrance composition and method for producing the same - Google Patents
Oil-in-water emulsified fragrance composition and method for producing the same Download PDFInfo
- Publication number
- JP4553607B2 JP4553607B2 JP2004061182A JP2004061182A JP4553607B2 JP 4553607 B2 JP4553607 B2 JP 4553607B2 JP 2004061182 A JP2004061182 A JP 2004061182A JP 2004061182 A JP2004061182 A JP 2004061182A JP 4553607 B2 JP4553607 B2 JP 4553607B2
- Authority
- JP
- Japan
- Prior art keywords
- oil
- fragrance
- composition
- silicone oil
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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- 239000003205 fragrance Substances 0.000 title claims description 89
- 239000000203 mixture Substances 0.000 title claims description 74
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- 238000004519 manufacturing process Methods 0.000 title claims description 11
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- DRRMRHKHTQRWMB-UHFFFAOYSA-N [3-(2-ethylhexanoyloxy)-2,2-bis(2-ethylhexanoyloxymethyl)propyl] 2-ethylhexanoate Chemical compound CCCCC(CC)C(=O)OCC(COC(=O)C(CC)CCCC)(COC(=O)C(CC)CCCC)COC(=O)C(CC)CCCC DRRMRHKHTQRWMB-UHFFFAOYSA-N 0.000 description 3
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- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 3
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- JXTPJDDICSTXJX-UHFFFAOYSA-N n-Triacontane Natural products CCCCCCCCCCCCCCCCCCCCCCCCCCCCCC JXTPJDDICSTXJX-UHFFFAOYSA-N 0.000 description 3
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- DSEKYWAQQVUQTP-XEWMWGOFSA-N (2r,4r,4as,6as,6as,6br,8ar,12ar,14as,14bs)-2-hydroxy-4,4a,6a,6b,8a,11,11,14a-octamethyl-2,4,5,6,6a,7,8,9,10,12,12a,13,14,14b-tetradecahydro-1h-picen-3-one Chemical compound C([C@H]1[C@]2(C)CC[C@@]34C)C(C)(C)CC[C@]1(C)CC[C@]2(C)[C@H]4CC[C@@]1(C)[C@H]3C[C@@H](O)C(=O)[C@@H]1C DSEKYWAQQVUQTP-XEWMWGOFSA-N 0.000 description 2
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Landscapes
- Fats And Perfumes (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Cosmetics (AREA)
Description
本発明は水中油型乳化香料組成物及びその製造方法、特に低粘度の水中油型乳化香料組成物及びその製造方法に関する。 The present invention relates to an oil-in-water emulsified fragrance composition and a method for producing the same, and particularly to a low-viscosity oil-in-water emulsified fragrance composition and a method for producing the same.
フレグランス組成物において、水を50質量%以上配合したような水系フレグランスは肌へ潤いを与える、あるいは肌への刺激が少ないという点で好まれている形態である。水系フレグランスとしては、香料を親水性界面活性剤で可溶化した透明可溶化系フレグランスや、香料を乳化した乳液系フレグランスが知られている。
前記透明可溶化系フレグランスにおいては、系の安定性は良いものの、香料を完全に溶解させるためには、界面活性剤を多量に配合する必要があり、べたつき・ぬめり等使用感触上の問題が生じることがある。また香りの持続性に問題が生じることもある。
一方、前記乳液系フレグランスとしては、使用感の良さ等から水中油型の乳化物が一般的に使用されている。
In the fragrance composition, an aqueous fragrance in which 50% by mass or more of water is blended is a preferred form in terms of moisturizing the skin or less irritation to the skin. As water-based fragrances, transparent solubilized fragrances in which fragrances are solubilized with hydrophilic surfactants and emulsion fragrances in which fragrances are emulsified are known.
In the transparent solubilizing fragrance, the stability of the system is good, but in order to completely dissolve the fragrance, it is necessary to add a large amount of a surfactant, which causes problems in use feeling such as stickiness and slime. Sometimes. There may also be problems with the persistence of the scent.
On the other hand, as the emulsion fragrance, an oil-in-water emulsion is generally used because of its good feeling of use.
しかしながら、フレグランスとして好ましい形態であるディスペンサー型にする場合、乳化物の粘度が高いと、均一に霧状に噴射することが困難であり、さらに使用するにつれて目詰まりを起こして噴射性が悪くなってしまうことがあった。
また、粘度を低くしようとしても、通常の界面活性剤や高分子を用いた乳化方法では、乳化粒子径が大きくなってしまい、クリーミングや乳化粒子の合一が起こりやすく、乳化組成物の安定性が悪いという問題が生じることがある。
本発明は前記従来技術の課題に鑑みなされたものであり、その目的は、使用感触及び乳化安定性に優れ、ディスペンサー仕様に耐えうる水系フレグランス及びその製造方法を提供することにある。
However, in the case of a dispenser type which is a preferable form as a fragrance, if the viscosity of the emulsion is high, it is difficult to inject uniformly in a mist form, and clogging occurs as the product is further used, resulting in poor injection properties. There was a case.
In addition, even when trying to reduce the viscosity, the emulsification method using a normal surfactant or polymer increases the particle size of the emulsified particles, which tends to cause creaming and coalescence of the emulsified particles, and the stability of the emulsified composition. May cause problems.
The present invention has been made in view of the above-described problems of the prior art, and an object thereof is to provide an aqueous fragrance excellent in use feeling and emulsification stability and capable of withstanding dispenser specifications, and a method for producing the same.
前記目的を達成するために本発明者等が検討を行った結果、親水性界面活性剤とシリコーン油とを用い、高圧乳化等により乳化粒子径を小さくした低粘度水中油型乳化組成物は、使用感触及び安定性に優れ、ディスペンサー仕様に耐えうることを見出し、本発明を完成するに至った。
すなわち、本発明の第一の主題は、香料0.5〜30質量%とシリコーン油とを含む油相と、
親水性界面活性剤と水とを含む水相と、を含有してなる組成物で、
香料:シリコーン油が2:3〜5:1、親水性界面活性剤:油相が1:2.4〜1:9であり、かつ香料及びシリコーン油の実質的全量が油滴に存在し、平均乳化粒子径が0.01〜0.2μmで、粘度が100mPa・s以下であることを特徴とする水中油型乳化香料組成物である。
As a result of investigations by the present inventors to achieve the above object, a low-viscosity oil-in-water emulsion composition using a hydrophilic surfactant and silicone oil and having a reduced emulsion particle size by high-pressure emulsification or the like, The present inventors have found that it is excellent in use feeling and stability and can withstand the dispenser specification, and has completed the present invention.
That is, the first subject of the present invention is an oil phase containing 0.5 to 30% by mass of a fragrance and silicone oil,
A composition comprising a hydrophilic surfactant and an aqueous phase containing water ,
Fragrance: silicone oil is 2: 3-5: 1, hydrophilic surfactant: oil phase is 1: 2.4-1: 9, and substantially all of the fragrance and silicone oil is present in the oil droplets; An oil-in-water emulsified fragrance composition having an average emulsified particle size of 0.01 to 0.2 μm and a viscosity of 100 mPa · s or less.
前記組成物において、親水性界面活性剤は、高級脂肪酸石鹸、ショ糖脂肪酸エステル、N−長鎖アシル酸性アミノ酸塩、ポリオキシエチレン硬化ヒマシ油、ポリオキシアルキレンアルキルエーテル、モノ脂肪酸ポリオキシエチレングリセリンからなる群より選択される1種又は2種以上であることが好適である。
また、シリコーン油は鎖状ポリシロキサン、環状ポリシロキサン、変性シリコーン油からなる群より選択される1種又は2種以上であることが好適である。
前記組成物において、さらに水相に多価アルコールを含有することが好適である。
また、さらに皮膜剤を含有することが好適である。
本発明の第二の主題は、香料0.5〜30質量%とシリコーン油とを含む油相と、
親水性界面活性剤と水とを含む水相とを混合攪拌し、香料:シリコーン油が2:3〜5:1、親水性界面活性剤:油相が1:2.4〜1:9であり、かつ香料及びシリコーン油の実質的全量が油滴に存在し、平均乳化粒子径が0.01〜0.2μmで、粘度が100mPa・s以下とすることを特徴とする水中油型乳化香料組成物の製造方法である。
In the composition, the hydrophilic surfactant is selected from higher fatty acid soap, sucrose fatty acid ester, N-long chain acyl acidic amino acid salt, polyoxyethylene hydrogenated castor oil, polyoxyalkylene alkyl ether, mono fatty acid polyoxyethylene glycerin. It is suitable that it is 1 type, or 2 or more types selected from the group which consists of.
The silicone oil is preferably one or more selected from the group consisting of chain polysiloxanes, cyclic polysiloxanes, and modified silicone oils.
In the composition, it is preferable that the aqueous phase further contains a polyhydric alcohol.
Further, it is preferable to further contain a film agent.
The second subject of the present invention is an oil phase comprising 0.5 to 30% by weight of perfume and silicone oil,
A hydrophilic surfactant and an aqueous phase containing water are mixed and stirred, and the fragrance: silicone oil is 2: 3 to 5: 1, and the hydrophilic surfactant: oil phase is 1: 2.4 to 1: 9. An oil-in-water emulsified fragrance characterized by having a substantial amount of the fragrance and silicone oil present in the oil droplets, having an average emulsified particle diameter of 0.01 to 0.2 μm and a viscosity of 100 mPa · s or less It is a manufacturing method of a composition.
本発明によれば、親水性界面活性剤とシリコーン油とを用い、高圧乳化等により乳化粒子径を小さくすることにより、使用感触及び安定性に優れる香料組成物を得ることができる。また、本発明にかかる香料組成物は、香りの持続性にも優れ、且つフレグランスとして扱いやすいディスペンサー仕様に耐え得るものとなる。
さらに、多価アルコールを配合すると、乳化粒子径が小さくなりやすい。また皮膜剤を配合すると、香りの持続性が良くなる。
According to the present invention, a fragrance composition excellent in use feeling and stability can be obtained by using a hydrophilic surfactant and silicone oil and reducing the emulsion particle diameter by high-pressure emulsification or the like. Moreover, the fragrance | flavor composition concerning this invention is excellent also in the sustainability of fragrance, and can endure the dispenser specification which is easy to handle as a fragrance.
Furthermore, when polyhydric alcohol is blended, the emulsified particle size tends to be small. Moreover, when a film agent is blended, the scent persistence is improved.
<香料>
本発明に用いる香料としては、動物又は植物より得られる天然香料と、化学的合成手段によって製造される合成香料、及びそれらの混合物である調合香料が挙げられ、特に限定されない。本発明においては、目的とする製品に応じて、これら香料の任意の一種または二種以上を用いることができる。
香料の配合量は、組成物全量に対して、通常0.5〜30質量%、より好ましくは1〜30質量%、さらに好ましくは2〜20質量%である。0.5質量%未満では、十分な香りの強さ・持続性が得られず、香料組成物として、十分な香りを得るには、1質量%以上であることが好ましい。また、30質量%を越える配合量は現実的に必要なく不経済である。
本発明の香料組成物には、上記香料の他に、シリコーン油、親水性界面活性剤、水を必須成分とする。
<Fragrance>
Examples of the fragrance used in the present invention include natural fragrances obtained from animals or plants, synthetic fragrances produced by chemical synthesis means, and blended fragrances that are mixtures thereof, and are not particularly limited. In the present invention, any one or two or more of these fragrances can be used depending on the intended product.
The compounding quantity of a fragrance | flavor is 0.5-30 mass% normally with respect to the composition whole quantity, More preferably, it is 1-30 mass%, More preferably, it is 2-20 mass%. If it is less than 0.5% by mass, sufficient strength and sustainability of the fragrance cannot be obtained, and in order to obtain a sufficient scent as a fragrance composition, it is preferably 1% by mass or more. Further, a blending amount exceeding 30% by mass is practically unnecessary and uneconomical.
The fragrance composition of the present invention contains silicone oil, a hydrophilic surfactant, and water as essential components in addition to the fragrance described above.
<シリコーン油>
シリコーン油は、ジメチルポリシロキサン、メチルフェニルポリシロキサン、メチルハイドロジェンポリシロキサン等の鎖状ポリシロキサン、オクタメチルシクロテトラシロキサン、デカメチルシクロペンタシロキサン、ドデカメチルシクロヘキサシロキサン、テトラメチルテトラハイドロジェンシクロテトラシロキサン等の環状ポリシロキサン、アミノ変性シリコーン油、エポキシ変性シリコーン油、エポキシ・ポリエーテル変性シリコーン油、ポリエーテル変性シリコーン油、カルボキシ変性シリコーン油、アルコール変性シリコーン油、アルキル変性シリコーン油、アンモニウム塩変性シリコーン油、フッ素変性シリコーン油等の変性シリコーン油等のシリコーン油が挙げられるが、好ましくは鎖状ポリシロキサン、環状ポリシロキサンである。
<Silicone oil>
Silicone oils are linear polysiloxanes such as dimethylpolysiloxane, methylphenylpolysiloxane, methylhydrogenpolysiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane, tetramethyltetrahydrogencyclotetra. Cyclic polysiloxanes such as siloxane, amino-modified silicone oil, epoxy-modified silicone oil, epoxy-polyether-modified silicone oil, polyether-modified silicone oil, carboxy-modified silicone oil, alcohol-modified silicone oil, alkyl-modified silicone oil, ammonium salt-modified silicone oil And silicone oils such as modified silicone oils such as fluorine-modified silicone oils, preferably chain polysiloxanes and cyclic polysiloxanes. It is.
<親水性界面活性剤>
親水性界面活性剤としては、高級脂肪酸石鹸、ショ糖脂肪酸エステル、N−長鎖アシル酸性アミノ酸塩、ポリオキシエチレン硬化ヒマシ油、ポリオキシアルキレンアルキルエーテル、モノ脂肪酸ポリオキシエチレングリセリンが挙げられるが、好ましくは高級脂肪酸石鹸、ショ糖脂肪酸エステル、N−長鎖アシル酸性アミノ酸塩、ポリオキシアルキレンアルキルエーテルであり、このうち、ポリオキシエチレン硬化ヒマシ油が安定性、使用感触等の点で非常に優れており、特に好ましい。
<Hydrophilic surfactant>
Examples of the hydrophilic surfactant include higher fatty acid soap, sucrose fatty acid ester, N-long chain acyl acidic amino acid salt, polyoxyethylene hydrogenated castor oil, polyoxyalkylene alkyl ether, mono fatty acid polyoxyethylene glycerin, Preferred are higher fatty acid soaps, sucrose fatty acid esters, N-long chain acyl acidic amino acid salts, and polyoxyalkylene alkyl ethers. Of these, polyoxyethylene hydrogenated castor oil is very excellent in terms of stability, feel in use, etc. It is particularly preferable.
高級脂肪酸石鹸としては、その高級脂肪酸が、直鎖状あるいは分岐鎖状の、飽和あるいは不飽和の、炭素数12〜22の脂肪酸であるものを用いることができ、このような高級脂肪酸としては、例えば、パルミチン酸、ステアリン酸、ベヘン酸等が挙げられる。高級脂肪酸石鹸の対イオンとしては、例えばカリウムイオン、ナトリウムイオン等の金属イオンが挙げられる。高級脂肪酸石鹸の炭素鎖長が長い方が、また鎖長の異なるものを組み合わせて用いることがより好ましい。 As the higher fatty acid soap, those whose higher fatty acid is a linear or branched, saturated or unsaturated fatty acid having 12 to 22 carbon atoms can be used. For example, palmitic acid, stearic acid, behenic acid and the like can be mentioned. Examples of the counter ion of the higher fatty acid soap include metal ions such as potassium ion and sodium ion. It is more preferable to use a higher fatty acid soap having a longer carbon chain length in combination with different chain lengths.
ショ糖脂肪酸エステルとしては、その脂肪酸が直鎖状あるいは分岐鎖状の、飽和あるいは不飽和の、炭素数12〜22のものを用いることができる。好ましくは、ショ糖脂肪酸エステル中のジエステルの純度が50%以上であるが、ジエステル以外のモノエステル及びトリエステルについて、モノ:トリ=1:3〜1:20の範囲にある場合には、ジエステルの純度は35%以上であればよい。このような高純度のジエステルは、市販のショ糖脂肪酸エステル(モノ、ジ、トリ体の混合物)を溶媒分別やカラムクロマトグラフィー等により精製して得ることができる(特開平7−25724参照)。 As the sucrose fatty acid ester, linear or branched, saturated or unsaturated fatty acid having 12 to 22 carbon atoms can be used. Preferably, the purity of the diester in the sucrose fatty acid ester is 50% or more, but when the monoester and the triester other than the diester are in the range of mono: tri = 1: 3 to 1:20, the diester The purity may be 35% or more. Such a high-purity diester can be obtained by purifying a commercially available sucrose fatty acid ester (mixture of mono-, di-, and tri-forms) by solvent fractionation, column chromatography, or the like (see JP-A-7-25724).
N−長鎖アシル酸性アミノ酸塩としては、その長鎖アシル基が、直鎖状あるいは分岐鎖状の、飽和あるいは不飽和の、炭素数12〜22、好ましくは16以上のものを用いることができる。このようなアシル基としては、例えば、ステアロイル基、パルミトイル基、ミリストイル基、ラウロイル基、ココイル基等が挙げられる。酸性アミノ酸としてはグルタミン酸、アスパラギン酸等が挙げられる。塩としては、ナトリウム、カリウム、トリエタノールアミン等の塩が挙げられる。好ましいものとしては、N−ラウロイルグルタミン酸ナトリウム、N−ラウロイルグルタミン酸カリウム、N−ミリストイルグルタミン酸ナトリウム、N−ミリストイルグルタミン酸カリウム、N−ステアロイルグルタミン酸ナトリウム、N−ステアロイルグルタミン酸カリウムが挙げられ、中でも、安定性に優れ、使用感触が良好であることから、N−ステアロイル−L−グルタミン酸ナトリウムが最も好ましい。 As the N-long chain acyl acidic amino acid salt, linear or branched, saturated or unsaturated, having 12 to 22, preferably 16 or more carbon atoms can be used. . Examples of such an acyl group include a stearoyl group, a palmitoyl group, a myristoyl group, a lauroyl group, and a cocoyl group. Examples of acidic amino acids include glutamic acid and aspartic acid. Examples of the salt include sodium, potassium, triethanolamine and the like. Preferable examples include sodium N-lauroyl glutamate, potassium N-lauroyl glutamate, sodium N-myristoyl glutamate, potassium N-myristoyl glutamate, sodium N-stearoyl glutamate, and potassium N-stearoyl glutamate. From the viewpoint of good use feeling, sodium N-stearoyl-L-glutamate is most preferable.
ポリオキシアルキレンアルキルエーテルとしては、例えば、ポリオキシエチレン(POE)C12−22アルキルエーテル、ポリオキシプロピレン(POP)C12−22アルキルエーテル等が挙げられる。そのPOE付加モル数としては、10〜30が好適である。好ましい例として、POE(15)オレイルエーテル等が挙げられる。
モノ脂肪酸POEグリセリンとしては、その脂肪酸が、直鎖状あるいは分岐鎖状の、飽和あるいは不飽和の、炭素数12〜22のものであり、HLB値としては8以上のものが好適である。具体例としては、イソステアリン酸ポリオキシエチレングリセリルが挙げられる。
Examples of the polyoxyalkylene alkyl ether include polyoxyethylene (POE) C12-22 alkyl ether, polyoxypropylene (POP) C12-22 alkyl ether, and the like. The POE addition mole number is preferably 10-30. Preferred examples include POE (15) oleyl ether.
As the mono fatty acid POE glycerin, the fatty acid is linear or branched, saturated or unsaturated, having 12 to 22 carbon atoms, and having an HLB value of 8 or more is preferable. Specific examples include polyoxyethylene glyceryl isostearate.
親水性界面活性剤の配合量は、通常、香料配合量に対して0.2〜3倍量、好ましくは0.5〜2倍量である。
また、親水性界面活性剤とシリコーン油との配合比は、本発明の効果を発揮する範囲で適宜調製可能である。例えば、ポリオキシエチレン硬化ヒマシ油:シリコーン油の場合には、通常モル比で1:0.5〜1:2、好ましくは1:1〜1:1.5である。
さらに油相と親水性界面活性剤との配合比は、通常質量比で油相/親水性界面活性剤=2.5程度であることが好ましい。
The compounding amount of the hydrophilic surfactant is usually 0.2 to 3 times, preferably 0.5 to 2 times the amount of the fragrance.
Moreover, the blending ratio of the hydrophilic surfactant and the silicone oil can be appropriately adjusted within a range where the effects of the present invention are exhibited. For example, in the case of polyoxyethylene hydrogenated castor oil: silicone oil, the molar ratio is usually 1: 0.5 to 1: 2, preferably 1: 1 to 1: 1.5.
Furthermore, the blending ratio of the oil phase to the hydrophilic surfactant is preferably about oil ratio / hydrophilic surfactant = 2.5 in general mass ratio.
<多価アルコール>
本発明の香料組成物には、さらに多価アルコールを配合すると、乳化粒子径が小さくなりやすいため好ましい。
多価アルコールとしては、例えば、2価のアルコール(例えば、エチレングリコール、プロピレングリコール、トリメチレングリコール、1,2-ブチレングリコール、1,3-ブチレングリコール、テトラメチレングリコール、2,3-ブチレングリコール、ペンタメチレングリコール、2-ブテン-1,4-ジオール、ヘキシレングリコール、オクチレングリコール等);3価のアルコール(例えば、グリセリン、トリメチロールプロパン等);4価アルコール(例えば、1,2,6-ヘキサントリオール等のペンタエリスリトール等);5価アルコール(例えば、キシリトール等);6価アルコール(例えば、ソルビトール、マンニトール等);多価アルコール重合体(例えば、ジエチレングリコール、ジプロピレングリコール、トリエチレングリコール、ポリプロピレングリコール、テトラエチレングリコール、ジグリセリン、ポリエチレングリコール、トリグリセリン、テトラグリセリン、ポリグリセリン等);2価のアルコールアルキルエーテル類(例えば、エチレングリコールモノメチルエーテル、エチレングリコールモノエチルエーテル、エチレングリコールモノブチルエーテル、エチレングリコールモノフェニルエーテル、エチレングリコールモノヘキシルエーテル、エチレングリコールモノ2-メチルヘキシルエーテル、エチレングリコールイソアミルエーテル、エチレングリコールベンジルエーテル、エチレングリコールイソプロピルエーテル、エチレングリコールジメチルエーテル、エチレングリコールジエチルエーテル、エチレングリコールジブチルエーテル等);2価アルコールアルキルエーテル類(例えば、ジエチレングリコールモノメチルエーテル、ジエチレングリコールモノエチルエーテル、ジエチレングリコールモノブチルエーテル、ジエチレングリコールジメチルエーテル、ジエチレングリコールジエチルエーテル、ジエチレングリコールブチルエーテル、ジエチレングリコールメチルエチルエーテル、トリエチレングリコールモノメチルエーテル、トリエチレングリコールモノエチルエーテル、プロピレングリコールモノメチルエーテル、プロピレングリコールモノエチルエーテル、プロピレングリコールモノブチルエーテル、プロピレングリコールイソプロピルエーテル、ジプロピレングリコールメチルエーテル、ジプロピレングリコールエチルエーテル、ジプロピレングリコールブチルエーテル等);2価アルコールエーテルエステル(例えば、エチレングリコールモノメチルエーテルアセテート、エチレングリコールモノエチルエーテルアセテート、エチレングリコールモノブチルエーテルアセテート、エチレングリコールモノフェニルエーテルアセテート、エチレングリコールジアジベート、エチレングリコールジサクシネート、ジエチレングリコールモノエチルエーテルアセテート、ジエチレングリコールモノブチルエーテルアセテート、プロピレングリコールモノメチルエーテルアセテート、プロピレングリコールモノエチルエーテルアセテート、プロピレングリコールモノプロピルエーテルアセテート、プロピレングリコールモノフェニルエーテルアセテート等);グリセリンモノアルキルエーテル(例えば、キシルアルコール、セラキルアルコール、バチルアルコール等);糖アルコール(例えば、ソルビトール、マルチトール、マルトトリオース、マンニトール、ショ糖、エリトリトール、グルコース、フルクトース、デンプン分解糖、マルトース、キシリトース、デンプン分解糖還元アルコール等);グリソリッド;テトラハイドロフルフリルアルコール;POE-テトラハイドロフルフリルアルコール;POP-ブチルエーテル;POP・POE-ブチルエーテル;トリポリオキシプロピレングリセリンエーテル;POP-グリセリンエーテル;POP-グリセリンエーテルリン酸;POP・POE-ペンタンエリスリトールエーテル、ポリグリセリン等を使用することができる。特にグリセリン、1,3-ブチレングリコール、ジプロピレングリコールが好適である。
<Polyhydric alcohol>
It is preferable to add a polyhydric alcohol to the fragrance composition of the present invention because the emulsified particle size tends to be small.
Examples of the polyhydric alcohol include divalent alcohols (for example, ethylene glycol, propylene glycol, trimethylene glycol, 1,2-butylene glycol, 1,3-butylene glycol, tetramethylene glycol, 2,3-butylene glycol, Pentamethylene glycol, 2-butene-1,4-diol, hexylene glycol, octylene glycol, etc.); trivalent alcohol (eg, glycerin, trimethylolpropane, etc.); tetravalent alcohol (eg, 1,2,6) -Pentaerythritol such as hexanetriol); pentavalent alcohol (for example, xylitol, etc.); hexavalent alcohol (for example, sorbitol, mannitol, etc.); polyhydric alcohol polymer (for example, diethylene glycol, dipropylene glycol, triethylene glycol, polypropylene Glycol, tetraethylene glycol, diglycerin, polyethylene glycol, triglycerin, tetraglycerin, polyglycerin, etc.); divalent alcohol alkyl ethers (for example, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, ethylene) Glycol monophenyl ether, ethylene glycol monohexyl ether, ethylene glycol mono 2-methylhexyl ether, ethylene glycol isoamyl ether, ethylene glycol benzyl ether, ethylene glycol isopropyl ether, ethylene glycol dimethyl ether, ethylene glycol diethyl ether, ethylene glycol dibutyl ether, etc.) ; Dihydric alcohol alkyl ester Tellurium (for example, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monobutyl ether, diethylene glycol dimethyl ether, diethylene glycol diethyl ether, diethylene glycol butyl ether, diethylene glycol methyl ethyl ether, triethylene glycol monomethyl ether, triethylene glycol monoethyl ether, propylene glycol monomethyl ether , Propylene glycol monoethyl ether, propylene glycol monobutyl ether, propylene glycol isopropyl ether, dipropylene glycol methyl ether, dipropylene glycol ethyl ether, dipropylene glycol butyl ether, etc.); divalent alcohol Ether esters (eg, ethylene glycol monomethyl ether acetate, ethylene glycol monoethyl ether acetate, ethylene glycol monobutyl ether acetate, ethylene glycol monophenyl ether acetate, ethylene glycol diazinate, ethylene glycol disuccinate, diethylene glycol monoethyl ether acetate, diethylene glycol) Monobutyl ether acetate, propylene glycol monomethyl ether acetate, propylene glycol monoethyl ether acetate, propylene glycol monopropyl ether acetate, propylene glycol monophenyl ether acetate, etc .; glycerin monoalkyl ethers (eg, xyl alcohol, ceralkyl alcohol) Sugar alcohol (for example, sorbitol, maltitol, maltotriose, mannitol, sucrose, erythritol, glucose, fructose, amylolytic sugar, maltose, xylitolose, amylolytic sugar reducing alcohol, etc.); Solid; Tetrahydrofurfuryl alcohol; POE-Tetrahydrofurfuryl alcohol; POP-Butyl ether; POP / POE-Butyl ether; Tripolyoxypropylene glycerin ether; POP-glycerin ether; POP-glycerin ether phosphate; POP / POE-pentane erythritol Ether, polyglycerin and the like can be used. Particularly preferred are glycerin, 1,3-butylene glycol, and dipropylene glycol.
本発明において、多価アルコールの配合量は特に限定されないが、香料組成物全量に対して、通常1〜20質量%、好ましくは5〜10質量%配合される。1質量%未満では、多価アルコールの添加効果が十分に発揮されず、20質量%を越えて配合しても配合量に見合った効果の増大が見込めず、またべたつきや希に刺激性などの問題を生じることがある。
さらに、本発明の香料組成物には、エタノールを配合すると、高温保存での安定性が特に高くなる。エタノールを配合する場合、配合量は組成物全量に対し1〜20質量%であることが好ましい。20質量%を超えると、エタノールの揮発にともない、保存中あるいは使用時の早い段階で揮発性の強い成分が揮発し、香調が甚だしく変化してしまう傾向にある。
In this invention, the compounding quantity of a polyhydric alcohol is although it does not specifically limit, Usually, 1-20 mass%, Preferably 5-10 mass% is mix | blended with respect to the fragrance | flavor composition whole quantity. If it is less than 1% by mass, the effect of adding polyhydric alcohol is not sufficiently exhibited, and even if it exceeds 20% by mass, an increase in effect commensurate with the blending amount cannot be expected, and stickiness, rarely irritation, etc. May cause problems.
Furthermore, when ethanol is added to the fragrance composition of the present invention, the stability at high temperature storage is particularly high. When blending ethanol, the blending amount is preferably 1 to 20% by mass with respect to the total amount of the composition. When it exceeds 20% by mass, with the volatilization of ethanol, a highly volatile component volatilizes during storage or at an early stage of use, and the fragrance tends to change drastically.
<皮膜剤>
本発明の香料組成物には、さらに皮膜剤を配合すると、香りの持続性が良くなるため好ましい。
本発明に用いる皮膜剤は、酢酸ビニルエマルジョン、ビニルピロリドン・酢酸ビニル共重合体、ポリ酢酸ビニルエマルジョン等の水系エマルジョン、カルボキシビニルポリマー、アクリル酸系・メタアクリル酸系樹脂、酢酸ビニル系樹脂、ポリビニルピロリドン系樹脂、セルロース誘導体樹脂、ポリビニルアルコール系樹脂、シリコーン系樹脂、メトキシエチレン無水マレイン酸共重合体、カチオン化セルロース、ポリ塩化ジメチルメチレン等、従来から用いられている公知のものを使用することができる。好ましくはポリビニルアルコール系樹脂である。
皮膜剤の配合量は、組成物全量に対し、0.1〜5質量%、好ましくは0.5〜2質量%である。0.1質量%未満では香りの持続効果が十分でなく、5質量%を超えると使用性が悪くなる傾向にある。
<Film agent>
It is preferable to add a film agent to the fragrance composition of the present invention because the fragrance sustainability is improved.
The coating agent used in the present invention is an aqueous emulsion such as vinyl acetate emulsion, vinyl pyrrolidone / vinyl acetate copolymer, polyvinyl acetate emulsion, carboxyvinyl polymer, acrylic acid / methacrylic acid resin, vinyl acetate resin, polyvinyl It is possible to use conventionally known ones such as pyrrolidone resins, cellulose derivative resins, polyvinyl alcohol resins, silicone resins, methoxyethylene maleic anhydride copolymers, cationized cellulose, polydimethylmethylene chloride and the like. it can. A polyvinyl alcohol resin is preferable.
The compounding quantity of a film agent is 0.1-5 mass% with respect to the composition whole quantity, Preferably it is 0.5-2 mass%. If it is less than 0.1% by mass, the effect of sustaining the fragrance is not sufficient, and if it exceeds 5% by mass, the usability tends to deteriorate.
上記必須成分である香料、シリコーン油の他に、適宜選択して他の油分を配合することにより、本願発明の水中油型乳化香料組成物をさらに安定な乳化物とすることができる。特に効果的なのはスクワラン及び/又はテトラオクタン酸ペンタエリスリチルである。
油相に配合される油分としては、特に限定されず、液状油分、固形油分、半固形油分の何れをも配合することができる。油分としては、例えば、アボガド油、ツバキ油、タートル油、マカデミアナッツ油、トウモロコシ油、ミンク油、オリーブ油、ナタネ油、卵黄油、ゴマ油、パーシック油、小麦胚芽油、サザンカ油、ヒマシ油、アマニ油、サフラワー油、綿実油、月見草油、エノ油、大豆油、落花生油、茶実油、カヤ油、コメヌカ油、シナギリ油、日本キリ油、ホホバ油、胚芽油、トリグリセリン、トリオクタン酸グリセリン、トリイソパルミチン酸グリセリン等の液体油脂;カカオ脂、ヤシ油、馬脂、硬化ヤシ油、パーム油、牛脂、羊脂、硬化牛脂、パーム核油、豚脂、牛骨脂、モクロウ核油、硬化油、牛脚脂、モクロウ、硬化ヒマシ油等の固形油脂;ミツロウ、カンデリラロウ、綿ロウ、カルナバロウ、ベイベリーロウ、イボタロウ、鯨ロウ、モンタンロウ、ヌカロウ、ラノリン、カポックロウ、酢酸ラノリン、液状ラノリン、サトウキビロウ、ラノリン脂肪酸イソプロピル、ラウリン酸ヘキシル、還元ラノリン、ジョジョバロウ、硬質ラノリン、セラックロウ、POEラノリンアルコールエーテル、POEラノリンアルコールアセテート、ラノリン脂肪酸ポリエチレングリコール、POE水素添加ラノリンアルコールエーテル等のロウ類;流動パラフィン、オゾケライト、スクワレン、プリスタン、パラフィン、セレシン、スクワラン、ワセリン、マイクロクリスタリンワックス等の炭化水素;ミリスチン酸イソプロピル、オクタン酸セチル、ミリスチン酸オクチルドデシル、パルミチン酸イソプロピル、ステアリン酸ブチル、ラウリン酸ヘキシル、ミリスチン酸ミリスチル、オレイン酸デシル、ジメチルオクタン酸ヘキシルデシル、乳酸セチル、乳酸ミリスチル、酢酸ラノリン、ステアリン酸イソセチル、イソステアレン酸イソセチル、12−ヒドロキシステアリル酸コレステリル、ジ−2−エチルヘキシル酸エチレングリコール、ジペンタエリスリトール脂肪酸エステル、モノイソステアリン酸N−アルキルグリコール、ジカプリン酸ネオペンチルグリコール、リンゴ酸ジイソステアリル、ジ−2−ヘプチルウンデカン酸グリセリン、トリ−2−エチルヘキシル酸トリメチロールプロパン、トリイソステアリン酸トリメチロールプロパン、テトラ−2−エチルヘキシル酸ペンタエリスリトール、トリ−2−エチルヘキシル酸グリセリン、トリイソステアリン酸トリメチロールプロパン、セチル−2−エチルヘキサノエート、2−エチルヘキシルパルミテート、トリミリスチン酸グリセリン、トリ−2−ヘプチルウンデカン酸グリセライド、ヒマシ油脂肪酸メチルエステル、オレイン酸オイル、セトステアリルアルコール、アセトグリセライド、パルミチン酸−2−ヘプチルウンデシル、アジピン酸ジイソプロピル、N−ラウロイル−L−グルタミン酸−2−オクチルドデシルエステル、アジピン酸ジ−2−ヘプチルウンデシル、エチルラウレート、セパチン酸ジ−2−エチルヘキシル、ミリスチン酸−2−ヘキシルデシル、パルミチン酸−2−ヘキシルデシル、アジピン酸−2−ヘキシルデシル、セバチル酸ジイソプロピル、コハク酸−2−エチルヘキシル、酢酸エチル、酢酸ブチル、酢酸アミル、クエン酸トリエチル、テトラオクタン酸ペンタエリスリチル等の合成エステル等が挙げられる。
The oil-in-water emulsified fragrance composition of the present invention can be made into a more stable emulsion by appropriately selecting and blending other oils in addition to the essential ingredients such as fragrance and silicone oil. Particularly effective are squalane and / or pentaerythrityl tetraoctanoate.
It does not specifically limit as an oil component mix | blended with an oil phase, Any liquid oil component, a solid oil component, and a semi-solid oil component can be mix | blended. Examples of oils include avocado oil, camellia oil, turtle oil, macadamia nut oil, corn oil, mink oil, olive oil, rapeseed oil, egg yolk oil, sesame oil, persic oil, wheat germ oil, sasanqua oil, castor oil, flaxseed oil, Safflower oil, cottonseed oil, evening primrose oil, eno oil, soybean oil, peanut oil, tea seed oil, kaya oil, rice bran oil, cinnagari oil, Japanese kiri oil, jojoba oil, germ oil, triglycerin, glyceryl trioctanoate, triiso Liquid fats such as glyceryl palmitate; cocoa butter, coconut oil, horse fat, hydrogenated coconut oil, palm oil, beef tallow, sheep fat, hardened beef tallow, palm kernel oil, pork tallow, beef bone fat, molasses kernel oil, hydrogenated oil, Solid fats such as beef leg fat, owl, hardened castor oil; beeswax, candelilla wax, cotton wax, carnauba wax, bayberry wax, ibota wax, whale wax, montanro , Nukarou, lanolin, kapok wax, lanolin acetate, liquid lanolin, sugarcane wax, lanolin fatty acid isopropyl, hexyl laurate, reduced lanolin, jojoballow, hard lanolin, shellac wax, POE lanolin alcohol ether, POE lanolin alcohol acetate, lanolin fatty acid polyethylene glycol, Waxes such as POE hydrogenated lanolin alcohol ether; hydrocarbons such as liquid paraffin, ozokerite, squalene, pristane, paraffin, ceresin, squalane, petrolatum, microcrystalline wax; isopropyl myristate, cetyl octanoate, octyldodecyl myristate, palmitic acid Isopropyl acid, butyl stearate, hexyl laurate, myristyl myristate, decyl oleate Hexyldecyl dimethyloctanoate, cetyl lactate, myristyl lactate, lanolin acetate, isocetyl stearate, isocetyl isostearate, cholesteryl 12-hydroxystearylate, ethylene glycol di-2-ethylhexylate, dipentaerythritol fatty acid ester, monoisostearic acid N -Alkyl glycol, neopentyl glycol dicaprate, diisostearyl malate, glycerin di-2-heptylundecanoate, trimethylolpropane tri-2-ethylhexylate, trimethylolpropane triisostearate, pentaerythritol tetra-2-ethylhexylate Glycerol tri-2-ethylhexylate, trimethylolpropane triisostearate, cetyl-2-ethylhexanoate, 2-ethyl Tilhexyl palmitate, glyceryl trimyristate, tri-2-heptylundecanoic acid glyceride, castor oil fatty acid methyl ester, oleic acid oil, cetostearyl alcohol, acetoglyceride, palmitic acid-2-heptylundecyl, diisopropyl adipate, N- Lauroyl-L-glutamic acid-2-octyldodecyl ester, di-2-heptylundecyl adipate, ethyl laurate, di-2-ethylhexyl sepatate, 2-hexyldecyl myristate, 2-hexyldecyl palmitate, Synthesis of adipic acid-2-hexyldecyl, diisopropyl sebacate, 2-ethylhexyl succinate, ethyl acetate, butyl acetate, amyl acetate, triethyl citrate, pentaerythrityl tetraoctanoate, etc. Tel and the like.
また、これらの油分に加えて、パーフルオロデカリン、パーフルオロヘキサン、トリパーフルオロ−n−ブチルアミン等のパーフルオロカーボンないしパーフルオロポリエーテル、ビタミンA及びその誘導体、ビタミンD及びその誘導体、ビタミンE及びその誘導体、ビタミンK及びその誘導体等のビタミン類、ステロール類等を配合することも可能である。
また、水に難溶性の物質を油相中に配合することも可能である。
In addition to these oils, perfluorocarbons or perfluoropolyethers such as perfluorodecalin, perfluorohexane, triperfluoro-n-butylamine, vitamin A and its derivatives, vitamin D and its derivatives, vitamin E and its Derivatives, vitamins such as vitamin K and its derivatives, sterols and the like can also be blended.
Moreover, it is also possible to mix | blend the water-insoluble substance in an oil phase.
本発明の香料組成物には、さらに、本発明の目的を損なわない範囲で、必要に応じて、通常化粧料等に配合される他の成分を配合することができる。
具体的には、例えば、クインスシード、カラギーナン、ペクチン、マンナン、カードラン、コンドロイチン硫酸、デンプン、ガラクタン、デルマタン硫酸、グリコーゲン、アラビアガム、ヘパラン硫酸、ヒアルロン酸、ヒアルロン酸ナトリウム、トラガントガム、ケラタン硫酸、コンドロイチン、キサンタンガム、ムコイチン硫酸、ヒドロキシエチルグアガム、カルボキシメチルグアガム、グアガム、デキストラン、ケラト硫酸、ローカストビーンガム、サクシノグルカン、カロニン酸、キチン、キトサン、カルボキシメチルキチン、寒天等の増粘剤;ブチルヒドロキシトルエン、トコフェロール、フィチン等の酸化防止剤;安息香酸、サリチル酸、ソルビン酸、パラオキシ安息香酸アルキルエステル、ヘキサクロロフェン等の抗菌剤;アシルサルコシン酸(例えばラウロイルサルコシンナトリウム)、グルタチオン、クエン酸、リンゴ酸、酒石酸、乳酸等の有機酸;ビタミンA及びその誘導体、ビタミンB6塩酸塩、ビタミンB6トリパルミテート、ビタミンB6ジオクタノエート、ビタミンB2及びその誘導体、ビタミンB12、ビタミンB15及びその誘導体等のビタミンB類、アスコルビン酸、アスコルビン酸硫酸エステル(塩)、アスコルビン酸リン酸エステル(塩)、アスコルビン酸ジパルミテート等のビタミンC類、α−トコフェロール、β−トコフェロール、δ−トコフェロール、ビタミンEアセテート等のビタミンE類、ビタミンD類、ビタミンH、パントテン酸、パンテチン等のビタミン類;ニコチン酸アミド、ニコチン酸ベンジル、γ−オリザノール、アラントイン、グリチルリチン酸(塩)、グリチルレチン酸及びその誘導体、ヒノキチオール、ビサボロール、ユーカルプトーン、チモール、イノシトール、サイコサポニン、ニンジンサポニン、ヘチマサポニン、ムクロジサポニン等のサポニン類、パントテニルエチルエーテル、エチニルエストラジオール、トラネキサム酸、アルブチン、セファランチン、プラセンタエキス等の各種薬剤;ギシギシ、クララ、コウホネ、オレンジ、セージ、ノコギリソウ、ゼニアオイ、センブリ、タイム、トウキ、トウヒ、バーチ、スギナ、ヘチマ、マロニエ、ユキノシタ、アルニカ、ユリ、ヨモギ、シャクヤク、アロエ、クチナシ、サワラ等の植物の抽出物;色素、モノラウリン酸ソルビタン、モノパルミチン酸ソルビタン、セスキオレイン酸ソルビタン、トリオレイン酸ソルビタン、モノラウリン酸ポリオキシエチレンソルビタン、モノステアリン酸ポリオキセチレンソルビタン、ポリエチレングリコールモノオレート、ポリオキシエチレンアルキルエーテル、ポリグリコールジエーテル、ラウロイルジエタノールアマイド、脂肪酸イソプロパノールアマイド、マルチトールヒドロキシ脂肪酸エーテル、アルキル化多糖、アルキルグルコシド、シュガーエステル等の非イオン性活性剤、ステアリルトリメチルアンモニウムクロライド、塩化ベンザルコニウム、ラウリルアミンオキサイド等のカチオン性界面活性剤、パルミチン酸ナトリウム、ラウリン酸ナトリウム、ラウリル酸ナトリウム、ラウリル硫酸カリウム、アルキル硫酸トリエタノールアミンエーテル、ロート油、リニアドデシルベンゼン硫酸、ポリオキシエチレン硬化ヒマシ油マレイン酸、アシルメチルタウリン等のアニオン性界面活性剤、両性界面活性剤、中和剤、酸化防止剤、保湿剤、防腐剤、顔料、薬剤等が配合可能である。
In the fragrance composition of the present invention, other components that are usually blended in cosmetics and the like can be blended as needed, as long as the object of the present invention is not impaired.
Specifically, for example, quince seed, carrageenan, pectin, mannan, curdlan, chondroitin sulfate, starch, galactan, dermatan sulfate, glycogen, gum arabic, heparan sulfate, hyaluronic acid, sodium hyaluronate, tragacanth gum, keratan sulfate, chondroitin , Xanthan gum, mucoitin sulfate, hydroxyethyl guar gum, carboxymethyl guar gum, guar gum, dextran, keratosulfuric acid, locust bean gum, succinoglucan, caronic acid, chitin, chitosan, carboxymethyl chitin, agar, etc .; , Antioxidants such as tocopherol and phytin; antibacterial agents such as benzoic acid, salicylic acid, sorbic acid, paraoxybenzoic acid alkyl ester, hexachlorophene; Organic acids such as sarcosine acid (eg, lauroyl sarcosine sodium), glutathione, citric acid, malic acid, tartaric acid, lactic acid; vitamin A and its derivatives, vitamin B6 hydrochloride, vitamin B6 tripalmitate, vitamin B6 dioctanoate, vitamin B2 and its Derivatives, vitamin B12 such as vitamin B12, vitamin B15 and derivatives thereof, ascorbic acid, ascorbic acid sulfate ester (salt), ascorbic acid phosphate ester (salt), vitamin C such as ascorbic acid dipalmitate, α-tocopherol, β -Vitamin E such as tocopherol, δ-tocopherol, vitamin E acetate, vitamin D, vitamin H, pantothenic acid, pantethine and the like; nicotinamide, benzyl nicotinate, γ-oryzanol, allanto In, glycyrrhizic acid (salt), glycyrrhetinic acid and its derivatives, hinokitiol, bisabolol, eucalptone, thymol, inositol, saikosaponin, carrot saponin, hechisaponin, muclodisaponin, etc. Various drugs such as tranexamic acid, arbutin, cephalanthin, placenta extract; borage, clara, corn, orange, sage, yarrow, mallow, assembly, thyme, toki, spruce, birch, sugina, loofah, maronier, yukinoshita, arnica, lily, Extracts of plants such as mugwort, peonies, aloe, gardenia, sawara; pigments, sorbitan monolaurate, sorbitan monopalmitate, sorbitan sesquioleate, birds Sorbitan oleate, polyoxyethylene sorbitan monolaurate, polyoxetylene sorbitan monostearate, polyethylene glycol monooleate, polyoxyethylene alkyl ether, polyglycol diether, lauroyl diethanol amide, fatty acid isopropanol amide, maltitol hydroxy fatty acid ether, alkyl Nonionic active agents such as modified polysaccharides, alkyl glucosides, sugar esters, cationic surfactants such as stearyltrimethylammonium chloride, benzalkonium chloride, laurylamine oxide, sodium palmitate, sodium laurate, sodium laurate, lauryl Potassium sulfate, alkyl sulfate triethanolamine ether, funnel oil, linear dodecylbenzene sulfate , Polyoxyethylene hardened castor oil maleic acid, anionic surfactants such as acyl methyl taurine, amphoteric surfactants, neutralizing agents, antioxidants, humectants, preservatives, pigments, drugs and the like can be blended.
本発明にかかる香料組成物は、例えば特許公報第2684188号に記載の高圧乳化方法に準じて製造できる。すなわち、上記必須成分等の混合分散液をホモミキサーよりも強力な剪断力をかけられる乳化機、例えば、マントンゴウリン、フレンチプレス、マイクロフルイタイザー、コロイドミル、超音波乳化機等で、強力な剪断力により処理し、平均乳化粒子径0.01〜0.2μm、粘度100mPa・s以下とする。マントンゴウリン、フレンチプレス、マイクロフルイタイザー等の高圧ホモジナイザーを用いる場合には、1,000psi以上、好ましくは3,000psi以上の圧力で乳化する。
このような乳化処理は、系全量を行ってもよいし、場合によっては一部を処理し、その後に水あるいは多価アルコール等の他の配合物により希釈してもよい。
The fragrance composition according to the present invention can be produced, for example, according to the high pressure emulsification method described in Japanese Patent Publication No. 2684188. That is, the emulsifier capable of applying a shear force stronger than the homomixer to the mixed dispersion of the above essential components, such as a manton gourin, a French press, a microfluidizer, a colloid mill, an ultrasonic emulsifier, etc. It processes by a shear force and it is set as an average emulsion particle diameter of 0.01-0.2 micrometer and a viscosity of 100 mPa * s or less. When a high-pressure homogenizer such as Manton gourin, French press, or microfluidizer is used, emulsification is performed at a pressure of 1,000 psi or more, preferably 3,000 psi or more.
Such an emulsification treatment may be carried out for the entire amount of the system, or may be partially treated in some cases and then diluted with other compounds such as water or polyhydric alcohol.
このような乳化処理により、乳化粒子径を0.01〜0.2μmまで微細にし、界面活性剤−香料−シリコーン油の実質的全量を水中油型乳化組成物の油滴に存在させることにより、100mPa・sという低粘度でも乳化安定性が非常に良好な水中油型乳化香料組成物が得られる。そして、この組成物はディスペンサー仕様にすることができる。
本発明の香料組成物の平均乳化粒子径は0.01〜0.2μm、好ましくは0.01〜0.08μmである。0.2μmを越えると、クリーミングを生じやすくなる。
粘度は、100mPa・s以下とすることが好適である。粘度が高くなると、ディスペンサー型の容器に充填した際に、噴霧性に影響を及ぼすことがある。
By such an emulsification treatment, the emulsified particle size is reduced to 0.01 to 0.2 μm, and a substantial amount of the surfactant-perfume-silicone oil is present in the oil droplets of the oil-in-water emulsion composition, An oil-in-water emulsified fragrance composition having very good emulsification stability even with a low viscosity of 100 mPa · s can be obtained. The composition can then be dispensed.
The average emulsified particle diameter of the fragrance composition of the present invention is 0.01 to 0.2 μm, preferably 0.01 to 0.08 μm. If it exceeds 0.2 μm, creaming tends to occur.
The viscosity is preferably 100 mPa · s or less. When the viscosity is high, sprayability may be affected when filling a dispenser type container.
本発明のフレグランス組成物は、中栓付きボトル容器あるいはディスペンサーにより霧状に噴霧して用いられる。ディスペンサー容器は、特に限定されず、通常用いられているものを使用することができる。
なお、前記特許公報第2684188号等において、親水性界面活性剤とシリコーン油とを用い、高圧乳化等の強力な剪断力により乳化粒子径を小さくして得られる組成物は、低粘度で経時安定性が良好であることが報告されているが、フレグランスのように香料を多量(1質量%以上)に配合する場合への応用についてはこれまで知られていなかった。
The fragrance composition of the present invention is used by spraying in a mist form with a bottle container with a stopper or a dispenser. The dispenser container is not particularly limited, and a commonly used one can be used.
In the above-mentioned Patent Publication No. 2684188 etc., a composition obtained by using a hydrophilic surfactant and silicone oil and reducing the emulsion particle size by a strong shearing force such as high-pressure emulsification is low in viscosity and stable over time. Although it has been reported that the property is good, its application to a case where a fragrance is blended in a large amount (1% by mass or more) like a fragrance has not been known so far.
以下、実施例を挙げて本発明をさらに詳しく説明する。本発明はこれらの実施例により限定されるものではない。配合量については特に断りのない限り質量%を示す。
まず、本発明で用いた試験方法について説明する。
<平均乳化粒子径測定方法>
エマルションの平均粒子径は、平均粒子径が1μm以上の場合は顕微鏡観察により測定した。平均粒子径が1μm以下の場合は動的光散乱法、具体的にはNICOMP−270(HIAC/ROYCO社製)により測定した。
Hereinafter, the present invention will be described in more detail with reference to examples. The present invention is not limited to these examples. Unless otherwise specified, the blending amount indicates mass%.
First, the test method used in the present invention will be described.
<Method for measuring average emulsified particle size>
The average particle diameter of the emulsion was measured by microscopic observation when the average particle diameter was 1 μm or more. When the average particle diameter was 1 μm or less, the measurement was performed by a dynamic light scattering method, specifically, NICOMP-270 (manufactured by HIAC / ROYCO).
<粘度測定方法>
芝浦システム(株)製「DIGITAL VISMETRON VDA(ローターNo.1)」を使用し、回転数12rpm、60sec.の条件で測定した。
<安定性評価>
試料をそれぞれ0℃、室温、37℃、50℃において4週間保存した後、状態の目視、及び乳化組成物の場合には乳化粒子径の測定により安定性の評価を行った。
◎:良好
○:若干の乳化粒子の合一が認められるものの、外観に問題ない
△:乳化粒子の合一が認められ、若干の油浮きも観察される
×:乳化粒子の合一が認められ、油相が分離する
<Viscosity measurement method>
Using “DIGITAL VISMETRON VDA (rotor No.1)” manufactured by Shibaura System Co., Ltd., rotating at 12 rpm, 60 sec. It measured on condition of this.
<Stability evaluation>
The samples were stored at 0 ° C., room temperature, 37 ° C., and 50 ° C. for 4 weeks, respectively, and then the stability was evaluated by visual observation of the state and, in the case of an emulsion composition, measurement of the emulsion particle diameter.
◎: Good ○: Some coalescence of emulsified particles is observed, but there is no problem in appearance △: Cohesion of emulsified particles is observed, and some oil floating is observed ×: Coalescence of emulsified particles is observed The oil phase separates
<香りの持続性評価>
試料の一定量を肌に塗布し、1時間後の香りの強さを専門パネルにより評価した。
◎ :強い
○ :やや強い
△ :どちらでもない(通常レベル)
× :弱い
<使用感評価>
20名の女性パネルの前腕に、試料を1.2mg/cm2塗布し、使用感触(べたつきのなさ、さっぱり感)の使用性試験を行ない、下記の通り評価した。
◎ :17名以上が良いと回答
○ :12名〜16名が良いと回答
△ :9名〜11名が良いと回答
× :5名〜8名が良いと回答
××:4名以下が良いと回答
<Scent sustainability evaluation>
A certain amount of the sample was applied to the skin, and the intensity of the scent after 1 hour was evaluated by a specialized panel.
◎: Strong ○: Slightly strong △: Neither (normal level)
×: weak <evaluation of use>
The sample was applied to the forearm of 20 female panels at 1.2 mg / cm 2, and a usability test (no stickiness, refreshing feeling) was performed, and evaluated as follows.
◎: 17 or more people are good ○ ○: 12 to 16 people are good △: 9 to 11 people are good ×: 5 to 8 people are good ××: 4 or less are good Answer
初めに、フローラル系調合香料A(※1)を用いて、下記表1の処方で香料を2質量%含む水中油型乳化組成物あるいは透明可溶化組成物を調製した。
(表1)
――――――――――――――――――――――――――――――――――――
試験例1 試験例2 試験例3
――――――――――――――――――――――――――――――――――――
水中油型 透明可溶化 水中油型
乳化組成物 組成物 乳化組成物
――――――――――――――――――――――――――――――――――――
水相部1
イオン交換水 15 残余 残余
グリセリン 3 − 3
ジプロピレングリコール 5 − 5
ポリオキシエチレン(60)硬化ヒマシ油 2 − 2
――――――――――――――――――――――――――――――――――――
油相部あるいは香料パーツ
フローラル系調合香料A 2 2 2
ジメチルポリシロキサン 3 −* 3
グリセリン − 0.5* −
ジプロピレングリコール − 3* −
ポリオキシエチレン(60)硬化ヒマシ油 − 3* −
――――――――――――――――――――――――――――――――――――
水相部2
イオン交換水 残余 − −
――――――――――――――――――――――――――――――――――――
平均乳化粒子径(μm) 0.04 − 1〜10
粘度(mPa・s) 10 12 15
安定性(0℃) ◎ ◎ ×
(室温) ◎ ◎ ×
(37℃) ◎ ◎ ×
(50℃) ○ ◎ ×
香りの持続性 ○ △ −
使用感(べたつきのなさ) ○ △ −
(さっぱり感) ○ △ −
――――――――――――――――――――――――――――――――――――
First, an oil-in-water emulsified composition or a transparent solubilized composition containing 2% by mass of a fragrance according to the formulation shown in Table 1 below was prepared using the floral blended fragrance A (* 1).
(Table 1)
――――――――――――――――――――――――――――――――――――
Test Example 1 Test Example 2 Test Example 3
――――――――――――――――――――――――――――――――――――
Oil-in-water type Transparent solubilization Oil-in-water type
Emulsified composition Composition Emulsified composition ――――――――――――――――――――――――――――――――――――
Water phase 1
Ion-exchanged water 15 Residue Residue Glycerin 3-3
Dipropylene glycol 5-5
Polyoxyethylene (60) hydrogenated castor oil 2-2
――――――――――――――――――――――――――――――――――――
Oil phase part or fragrance part Floral-type compound fragrance A 2 2 2
Dimethylpolysiloxane 3-* 3
Glycerin-0.5 *-
Dipropylene glycol-3 *-
Polyoxyethylene (60) hydrogenated castor oil-3 *-
――――――――――――――――――――――――――――――――――――
Water phase 2
Ion exchange water Residual--
――――――――――――――――――――――――――――――――――――
Average emulsified particle size (μm) 0.04-1 to 10
Viscosity (mPa · s) 10 12 15
Stability (0 ℃) ◎ ◎ ×
(Room temperature) ◎ ◎ ×
(37 ℃) ◎ ◎ ×
(50 ℃) ○ ◎ ×
Aroma persistence ○ △ −
Feel (no stickiness) ○ △ −
(Refreshing feeling) ○ △ −
――――――――――――――――――――――――――――――――――――
(製造方法)
試験例1:油相部を攪拌溶解後、水相部1を70℃で加熱溶解したものに攪拌しながら添加し、乳化した。この乳液を7,000psiの圧力下、70〜80℃において高圧ホモジナイザーを用いて乳化した後、水相部2を添加混合して冷却し、水中油型乳化組成物を得た。
試験例2:グリセリン、ジプロピレングリコールにポリオキシエチレン(60)硬化ヒマシ油を撹拌混合し、さらに香料を加えて香料パーツとする。水相部1に上記香料パーツを加え、撹拌混合し、透明可溶化組成物を得た(*:透明可溶化組成物の場合、可溶化が困難なシリコーン油は配合せず、さらに、使用感を損ねないため多価アルコールをできる限り減量して通常調製した)。
試験例3:油相部を攪拌溶解後、水相部1にホモミキサー処理(9,000rpm)を行ないながら添加して乳化後、脱気・冷却し、水中油型乳化組成物を得た。
(Production method)
Test Example 1: The oil phase part was stirred and dissolved, and then added to the water phase part 1 heated and dissolved at 70 ° C. with stirring, and emulsified. The emulsion was emulsified using a high-pressure homogenizer at 70 to 80 ° C. under a pressure of 7,000 psi, and then the aqueous phase 2 was added and mixed to cool to obtain an oil-in-water emulsion composition.
Test Example 2: Polyoxyethylene (60) hydrogenated castor oil is stirred and mixed with glycerin and dipropylene glycol, and a fragrance is added to obtain a fragrance part. The above fragrance parts were added to the water phase part 1 and mixed by stirring to obtain a transparent solubilized composition (*: In the case of a transparent solubilized composition, a silicone oil that is difficult to solubilize is not blended, and further, feeling of use In general, the amount of polyhydric alcohol was reduced as much as possible.
Test Example 3: The oil phase part was stirred and dissolved, and then added to the water phase part 1 while performing homomixer treatment (9,000 rpm), emulsified, degassed and cooled to obtain an oil-in-water emulsion composition.
(※1)フローラル系調合香料A
1.オレンジ油 5
2.ジハイドロミルセノール 5
3.リナロール 7
4.酢酸リナリル 3
5.酢酸ベンジル 5
6.ローズ ベース 15
7.ヘキシルシンナムアルデヒド 5
8.メチル ヨノン ガンマ 5
9.ガラクソライド 10
10.エディオン 20
11.リリアール 10
12.その他香料 10
―――――――――――――――――――――
合計 100
(* 1) Floral-type blended fragrance A
1. Orange oil 5
2. Dihydromilsenol 5
3. Linalool 7
4). Linalyl acetate 3
5). Benzyl acetate 5
6). Rose base 15
7). Hexylcinnamaldehyde 5
8). Methyl Yonon Gamma 5
9. Garaxoride 10
10. Edion 20
11. Lilianal 10
12 Other fragrances 10
―――――――――――――――――――――
Total 100
試験例2は、香料を可溶化することによって調製された透明可溶化組成物である。この組成物は、乳化安定性は良いものの、使用感が悪かった。また香りの持続性も劣るものであった。
これに対し、試験例1は親水性界面活性剤及びシリコーン油を用い、高圧乳化により調製された水中油型乳化組成物である。この組成物は、乳化粒子径及び粘度が小さく、且つ乳化安定性が高く、且つべたつきがなく、さっぱりとした良好な使用感を有していた。また、試験例2の透明可溶化組成物に比べて香りの持続性が高いものであった。
また試験例3は、組成は試験例1と同じであるが、通常の乳化方法により調製された水中油型乳化組成物である。この組成物は、乳化粒子の合一が認められ、油相が分離し、安定性が非常に悪いものであった。
Test Example 2 is a transparent solubilized composition prepared by solubilizing a fragrance. Although this composition had good emulsification stability, the feeling of use was poor. Moreover, the persistence of the fragrance was inferior.
In contrast, Test Example 1 is an oil-in-water emulsion composition prepared by high-pressure emulsification using a hydrophilic surfactant and silicone oil. This composition had a small emulsion particle size and viscosity, high emulsion stability, no stickiness, and a refreshing and good feeling of use. Moreover, compared with the transparent solubilized composition of Test Example 2, the fragrance persistence was high.
Test Example 3 is an oil-in-water emulsion composition having the same composition as Test Example 1, but prepared by a normal emulsification method. In this composition, coalescence of emulsified particles was observed, the oil phase was separated, and the stability was very poor.
香料は他の油分と異なり、種類により極性が大きく異なる。フローラル系調合香料Aにおいても、極性の低いオレンジ油から極性の高いローズベースまで、極性が異なる多様な香料を含んでいる。よって、従来の乳化方法では良好な安定性が得られなかった。しかしながら、本発明の製造方法によれば、極性が異なる多様な香料を含んでいるにもかかわらず、安定した乳化系を形成することができることが確認された。 Unlike other oils, fragrances vary greatly in polarity. Floral-based blended fragrance A also contains a variety of fragrances having different polarities, from orange oil with low polarity to rose base with high polarity. Therefore, good stability cannot be obtained by the conventional emulsification method. However, according to the production method of the present invention, it was confirmed that a stable emulsification system can be formed even though various perfumes having different polarities are included.
次に、香料の配合量を変えて検討を行った。下記表2の処方で試験例1の製法に準じて、香料を7質量%含む水中油型乳化組成物を調製した。
(表2)
――――――――――――――――――――――――――――――――――――――
試験例4 試験例5 試験例6
――――――――――――――――――――――――――――――――――――――
水相部1
イオン交換水 50 50 50
グリセリン 5 − −
ジプロピレングリコール 5 2 2
1,3−ブチレングリコール 10 5 5
ポリオキシエチレン(60)硬化ヒマシ油 7 7 7
――――――――――――――――――――――――――――――――――――――
油相部
フローラル系調合香料A 7 7 7
ジメチルポリシロキサン 10 10 8
テトラオクタン酸ペンタエリスリチル − − 2
――――――――――――――――――――――――――――――――――――――
水相部2
イオン交換水 残余 残余 残余
――――――――――――――――――――――――――――――――――――――
平均乳化粒子径(μm) 0.03 0.04 0.04
粘度(mPa・s) 40 30 30
乳化安定性(0℃) ◎ ◎ ◎
(室温) ◎ ◎ ◎
(37℃) ◎ ◎ ◎
(50℃) ◎ ○ ○
香りの持続性 ○ ○ ◎
使用感(べたつきのなさ) △ ○ ○
(さっぱり感) △ ○ ○
――――――――――――――――――――――――――――――――――――――
香料を7質量%配合した場合においても、界面活性剤及びシリコーン油の配合量は増大するが、多価アルコール及び/又は油分の組み合わせ・配合量を検討することにより、使用感触および安定性に優れた水中油型乳化組成物が得られた。
Next, it examined by changing the compounding quantity of a fragrance | flavor. An oil-in-water emulsion composition containing 7% by mass of a fragrance was prepared according to the production method of Test Example 1 with the formulation shown in Table 2 below.
(Table 2)
――――――――――――――――――――――――――――――――――――――
Test Example 4 Test Example 5 Test Example 6
――――――――――――――――――――――――――――――――――――――
Water phase 1
Ion exchange water 50 50 50
Glycerin 5--
Dipropylene glycol 5 2 2
1,3-butylene glycol 10 5 5
Polyoxyethylene (60) hydrogenated castor oil 7 7 7
――――――――――――――――――――――――――――――――――――――
Oil phase part floral blended fragrance A 7 7 7
Dimethylpolysiloxane 10 10 8
Pentaerythrityl tetraoctanoate --2
――――――――――――――――――――――――――――――――――――――
Water phase 2
Ion-exchanged water Residual Residual Residual Residual Residue ――――――――――――――――――――――――――――――――――――――
Average emulsified particle size (μm) 0.03 0.04 0.04
Viscosity (mPa · s) 40 30 30
Emulsification stability (0 ℃) ◎ ◎ ◎
(Room temperature) ◎ ◎ ◎
(37 ℃) ◎ ◎ ◎
(50 ℃) ◎ ○ ○
Aroma persistence ○ ○ ◎
Usability (no stickiness) △ ○ ○
(Refreshing feeling) △ ○ ○
――――――――――――――――――――――――――――――――――――――
Even when 7% by mass of the fragrance is blended, the blending amount of the surfactant and the silicone oil increases. However, by examining the combination and blending amount of the polyhydric alcohol and / or the oil, it is excellent in use feeling and stability. An oil-in-water emulsion composition was obtained.
さらに、フローラル系調合香料B(※2)に対して、下記表3の処方で試験例1の製法に準じて水中油型乳化組成物を調製した。
(表3)
―――――――――――――――――――――――――――――――――――――
試験例7 試験例8 試験例9
―――――――――――――――――――――――――――――――――――――
水相部1
イオン交換水 25 25 25
グリセリン 4 4 4
ジプロピレングリコール 2 2 2
ポリオキシエチレン(60)硬化ヒマシ油 2 2 2
N−ステアロイルグルタミン酸Na 0.03 0.03 0.03
―――――――――――――――――――――――――――――――――――――
油相部
フローラル系調合香料B 2 2 2
ジメチルポリシロキサン 2.9 2.9 2.9
スクワラン 0.1 0.1 0.1
―――――――――――――――――――――――――――――――――――――
水相部2
イオン交換水 残余 残余 残余
エタノール − 10 −
ポリビニルアルコール(低粘度タイプ) − − 1
―――――――――――――――――――――――――――――――――――――
平均乳化粒子径(μm) 0.04 0.05 0.04
粘度(mPa・s) 10 12 20
乳化安定性(0℃) ◎ ◎ ◎
(室温) ◎ ◎ ◎
(37℃) ○ ◎ ◎
(50℃) ○ ◎ ○
香りの持続性 ○ ○ ◎
使用感(べたつきのなさ) ○ ○ ○
(さっぱり感) ○ ○ ○
―――――――――――――――――――――――――――――――――――――
試験例7〜9の何れも乳化安定性、香りの持続性及び使用感触が良好であった。また、試験例8はさらにエタノールを配合しているので、高温保存で安定性がさらに高いものとなった。また、試験例9は皮膜剤(ポリビニルアルコール)を配合しているので、香りの持続性がさらに高いものとなった。
Furthermore, an oil-in-water emulsion composition was prepared according to the production method of Test Example 1 with the formulation shown in Table 3 below with respect to the floral blended fragrance B (* 2).
(Table 3)
―――――――――――――――――――――――――――――――――――――
Test Example 7 Test Example 8 Test Example 9
―――――――――――――――――――――――――――――――――――――
Water phase 1
Ion exchange water 25 25 25
Glycerin 4 4 4
Dipropylene glycol 2 2 2
Polyoxyethylene (60) hydrogenated castor oil 2 2 2
N-stearoyl glutamate Na 0.03 0.03 0.03
―――――――――――――――――――――――――――――――――――――
Oil phase part floral blending fragrance B 2 2 2
Dimethylpolysiloxane 2.9 2.9 2.9
Squalane 0.1 0.1 0.1
―――――――――――――――――――――――――――――――――――――
Water phase 2
Ion-exchanged water Residue Residue Residue Ethanol − 10 −
Polyvinyl alcohol (low viscosity type) − − 1
―――――――――――――――――――――――――――――――――――――
Average emulsified particle size (μm) 0.04 0.05 0.04
Viscosity (mPa · s) 10 12 20
Emulsification stability (0 ℃) ◎ ◎ ◎
(Room temperature) ◎ ◎ ◎
(37 ℃) ○ ◎ ◎
(50 ℃) ○ ◎ ○
Aroma persistence ○ ○ ◎
Feeling of use (no stickiness) ○ ○ ○
(Refreshing feeling) ○ ○ ○
―――――――――――――――――――――――――――――――――――――
In all of Test Examples 7 to 9, the emulsion stability, the scent durability and the feeling of use were good. Moreover, since Test Example 8 further blended ethanol, the stability was further enhanced by high temperature storage. Moreover, since the test example 9 mix | blended the film | membrane agent (polyvinyl alcohol), the sustainability of fragrance became still higher.
(※2)フローラル系調合香料B
1.オレンジ油 4
2.レモン油 3
3.ジハイドロミルセノール 3
4.リナロール 15
5.ローズ ベース 10
6.ターピネオール 5
7.メチル ヨノン ガンマ 5
8.ベータ ヨノン 5
9.ヴェルトフィックス 10
10.エディオン 15
11.フロローサ(FLOROSA、QUEST社) 20
12.その他香料 5
―――――――――――――――――――――――
合計 100
(* 2) Floral-type blended fragrance B
1. Orange oil 4
2. Lemon oil 3
3. Dihydromilsenol 3
4). Linaroll 15
5). Rose base 10
6). Turpineol 5
7). Methyl Yonon Gamma 5
8). Beta Yonon 5
9. Weltfix 10
10. Edion 15
11. Florosa (FLOROSA, QUEST) 20
12 Other fragrances 5
―――――――――――――――――――――――
Total 100
本発明にかかる水中油型乳化香料組成物の実施例を以下に示す。いずれの組成物も使用感触及び乳化安定性に優れ、ディスペンサー仕様に耐えうるものであった。また平均乳化粒子径は0.01〜0.2μm、粘度が100mPa・s以下であった。
―――――――――――――――――――――――――――――――――――――
試験例10 試験例11 試験例12
―――――――――――――――――――――――――――――――――――――
水相部1
イオン交換水 50 50 50
グリセリン 4 8 8
ジプロピレングリコール 2 − −
ポリオキシエチレン(60)硬化ヒマシ油 4 4 4
N−ステアロイルグルタミン酸Na 0.03 0.03 0.03
―――――――――――――――――――――――――――――――――――――
油相部
香料B 10 20 30
ジメチルポリシロキサン 5 10 5
メチルフェニルポリシロキサン 5 1 1
デカメチルサイクロペンタシロキサン 5 − −
―――――――――――――――――――――――――――――――――――――
水相部2
イオン交換水 残余 残余 残余
―――――――――――――――――――――――――――――――――――――
平均乳化粒子径(μm) 0.15 0.17 0.20
粘度(mPa・s) 20 30 55
乳化安定性(0℃) ○ ○ ○
(室温) ○ ○ ○
(37℃) ○ ○ ○
(50℃) ○ ○ ○
香りの持続性 ○ ○ ○
使用感(べたつきのなさ) ○ ○ ○
(さっぱり感) ○ ○ ○
―――――――――――――――――――――――――――――――――――――
(製造方法)
油相部を攪拌溶解後、水相部1を70℃で加熱溶解したものに攪拌しながら添加し、乳化した。この乳液を7,000psiの圧力下、70〜80℃において高圧ホモジナイザーを用いて乳化した後、水相部2を添加混合して冷却し、水中油型乳化組成物を得た。
Examples of the oil-in-water emulsified fragrance composition according to the present invention are shown below. All the compositions were excellent in use feeling and emulsion stability, and could withstand the dispenser specifications. The average emulsified particle size was 0.01 to 0.2 μm, and the viscosity was 100 mPa · s or less.
―――――――――――――――――――――――――――――――――――――
Test Example 10 Test Example 11 Test Example 12
―――――――――――――――――――――――――――――――――――――
Water phase 1
Ion exchange water 50 50 50
Glycerin 4 8 8
Dipropylene glycol 2--
Polyoxyethylene (60) hydrogenated castor oil 4 4 4
N-stearoyl glutamate Na 0.03 0.03 0.03
―――――――――――――――――――――――――――――――――――――
Oil phase fragrance B 10 20 30
Dimethylpolysiloxane 5 10 5
Methylphenylpolysiloxane 5 1 1
Decamethylcyclopentasiloxane 5-
―――――――――――――――――――――――――――――――――――――
Water phase 2
Ion-exchanged water Residual Residual Residual Residual Residual Residue
Average emulsified particle size (μm) 0.15 0.17 0.20
Viscosity (mPa · s) 20 30 55
Emulsification stability (0 ° C) ○ ○ ○
(Room temperature) ○ ○ ○
(37 ℃) ○ ○ ○
(50 ℃) ○ ○ ○
Aroma persistence ○ ○ ○
Feeling of use (no stickiness) ○ ○ ○
(Refreshing feeling) ○ ○ ○
―――――――――――――――――――――――――――――――――――――
(Production method)
After stirring and dissolving the oil phase part, the aqueous phase part 1 was added with stirring to an aqueous solution at 70 ° C. and emulsified. The emulsion was emulsified using a high-pressure homogenizer at 70 to 80 ° C. under a pressure of 7,000 psi, and then the aqueous phase 2 was added and mixed to cool to obtain an oil-in-water emulsion composition.
Claims (6)
親水性界面活性剤と水とを含む水相と、を含有してなる組成物で、
香料:シリコーン油が質量比で2:3〜5:1、親水性界面活性剤:油相が質量比で1:2.4〜1:9であり、かつ香料及びシリコーン油の実質的全量が油滴に存在し、
平均乳化粒子径が0.01〜0.2μmで、粘度が100mPa・s以下であることを特徴とする水中油型乳化香料組成物。 An oil phase containing 0.5 to 30% by mass of a fragrance and silicone oil;
A composition comprising a hydrophilic surfactant and an aqueous phase containing water ,
Perfume: silicone oil is in a mass ratio of 2: 3 to 5: 1, hydrophilic surfactant: oil phase is in a mass ratio of 1: 2.4 to 1: 9, and substantially all of the perfume and silicone oil is Present in the oil droplets,
An oil-in-water emulsified fragrance composition having an average emulsified particle diameter of 0.01 to 0.2 μm and a viscosity of 100 mPa · s or less.
親水性界面活性剤と水とを含む水相とを混合攪拌し、香料:シリコーン油が2:3〜5:1、親水性界面活性剤:油相が1:2.4〜1:9であり、かつ香料及びシリコーン油の実質的全量が油滴に存在し、平均乳化粒子径が0.01〜0.2μmで、粘度が100mPa・s以下とすることを特徴とする水中油型乳化香料組成物の製造方法。 An oil phase containing 0.5 to 30% by mass of a fragrance and silicone oil;
A hydrophilic surfactant and an aqueous phase containing water are mixed and stirred, and the fragrance: silicone oil is 2: 3 to 5: 1, and the hydrophilic surfactant: oil phase is 1: 2.4 to 1: 9. An oil-in-water emulsified fragrance characterized by having a substantial amount of the fragrance and silicone oil present in the oil droplets, having an average emulsified particle diameter of 0.01 to 0.2 μm and a viscosity of 100 mPa · s or less A method for producing the composition.
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JPH01293131A (en) * | 1988-05-17 | 1989-11-27 | Shiseido Co Ltd | Microemulsion |
JPH0640877A (en) * | 1992-05-29 | 1994-02-15 | Quest Internatl Bv | Aqueous perfumed oil micro-emulsion |
JPH08231980A (en) * | 1995-02-22 | 1996-09-10 | Shiseido Co Ltd | Perfumary composition |
JPH09505565A (en) * | 1993-11-02 | 1997-06-03 | ジボーダン − ルール (アンテルナシヨナル)ソシエテ アノニム | Fragrance compound |
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JPH01293131A (en) * | 1988-05-17 | 1989-11-27 | Shiseido Co Ltd | Microemulsion |
JPH0640877A (en) * | 1992-05-29 | 1994-02-15 | Quest Internatl Bv | Aqueous perfumed oil micro-emulsion |
JPH09505565A (en) * | 1993-11-02 | 1997-06-03 | ジボーダン − ルール (アンテルナシヨナル)ソシエテ アノニム | Fragrance compound |
JPH08231980A (en) * | 1995-02-22 | 1996-09-10 | Shiseido Co Ltd | Perfumary composition |
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