JPS63107740A - Preparation of oil-in-water-type emulsion - Google Patents

Preparation of oil-in-water-type emulsion

Info

Publication number
JPS63107740A
JPS63107740A JP61252455A JP25245586A JPS63107740A JP S63107740 A JPS63107740 A JP S63107740A JP 61252455 A JP61252455 A JP 61252455A JP 25245586 A JP25245586 A JP 25245586A JP S63107740 A JPS63107740 A JP S63107740A
Authority
JP
Japan
Prior art keywords
water
oil
emulsion
mixed
polyhydric alcohol
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.)
Pending
Application number
JP61252455A
Other languages
Japanese (ja)
Inventor
Hiromichi Sagiya
鷺谷 広道
Yoshikazu Hirai
義和 平井
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Pola Orbis Holdings Inc
Original Assignee
Pola Chemical Industries Inc
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Pola Chemical Industries Inc filed Critical Pola Chemical Industries Inc
Priority to JP61252455A priority Critical patent/JPS63107740A/en
Publication of JPS63107740A publication Critical patent/JPS63107740A/en
Pending legal-status Critical Current

Links

Classifications

    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/04Dispersions; Emulsions
    • A61K8/06Emulsions
    • A61K8/062Oil-in-water emulsions
    • 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
    • A61K2800/20Chemical, physico-chemical or functional or structural properties of the composition as a whole
    • A61K2800/26Optical properties
    • A61K2800/262Transparent; Translucent

Abstract

PURPOSE:To enhance the stability of an oil-in-water-type emulsion, by a method wherein a solution mixture of water-soluble polyhydric alcohol and water is added to a mixed phase of a surfactant and an oil phase to form a gel like or transparent liquid composition which is, in turn, mixed with an aqueous phase. CONSTITUTION:A surfactant and an oil phase are mixed and a solution mixture of water-soluble polyhydric alcohol and water is added to the resulting mixed phase to form a gel like or transparent liquid composition which is, in turn, mixed with an aqueous phase to prepare an oil-in-water-type emulsion. The mixing amount of the surfactant is pref. 7% or more by wt. of the amount of the oil phase and the mixing wt. ratio of water-soluble polyhydric alcohol and water is pref. within a range of 8:2-2:8. As the oil phase, there are animal and vegetable oils or fats, waxes and hydrocarbons and, as water-soluble polyhydric alcohol, there are ethylene glycol, 1,3-butane diol or the like.

Description

【発明の詳細な説明】 本発明は、新規な水中油型エマルジョンの製造方法に関
するものである。更に詳しくは、本発明は従来乳化力が
弱く均−且つ安定なエマルジ曹ンを調製することが困難
であった界面活性剤を用いた場合でも、均−且つ安定な
エマルジッン状態を維持し得る全く新しい水中油型エマ
ルジョンの製造方法に係るものである。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a novel method for producing oil-in-water emulsions. More specifically, the present invention provides a complete emulsion that can maintain a uniform and stable emulsion state even when using a surfactant that has conventionally been difficult to prepare a uniform and stable emulsion with weak emulsifying power. This invention relates to a new method for producing an oil-in-water emulsion.

従来、安定な水中油型(以下0/W型)エマルジ冒ンを
製造する方法としては、石ケンを乳化剤とする場合は同
時乳化法が、また非イオン界面活性剤を用いる場合には
反転乳化法や自己乳化法が用いられてきた。このうち非
イオン界面活性剤は皮膚刺激が低いため、化粧品用乳化
剤として広く利用されている。
Conventionally, methods for producing stable oil-in-water type (0/W type) emulsions include simultaneous emulsification when soap is used as an emulsifier, and inverse emulsification when nonionic surfactants are used. method and self-emulsification method have been used. Among these, nonionic surfactants are widely used as cosmetic emulsifiers because they cause less skin irritation.

この非イオン界面活性剤を用いる乳化法のうち、反転乳
化法は乳化剤を先ず油相に溶解し、次いでこれに水を少
量づつ加えることにより、油連続相から反転時の液晶相
を形成させた後、さらに水を加えて0/W型エマルジ冒
ンとする方法で最も一般的なものである。
Among the emulsification methods using nonionic surfactants, the inversion emulsification method involves first dissolving the emulsifier in the oil phase, and then adding water little by little to form a liquid crystal phase during inversion from the oil continuous phase. This is the most common method in which water is then added to evaporate the O/W emulsion.

一方、自己乳化法は界面活性剤の親水性・親油性バラン
ス(HLB )を、油水界面張力が充分に小さくなる様
に調整した乳化剤を油相中に含有させ、これに水を加え
ることKよって自然乳化を起こさせる様にした方法であ
る。
On the other hand, in the self-emulsification method, the hydrophilicity/lipophilicity balance (HLB) of the surfactant is adjusted so that the oil-water interfacial tension is sufficiently small, and an emulsifier is contained in the oil phase, and water is added to this. This method is designed to cause natural emulsification.

然しなから、最近は人体に対する安全性をより向上させ
るため、より高分子化された乳化剤が用いられる様にな
りてきており、その結果として分子量の増大に伴ない乳
化力が低下し、これまでの方法では均一なO/Wlエマ
ルジ買ンが製造できない場合も生じる様になってきた。
However, recently, in order to further improve safety for the human body, emulsifiers with higher molecular weight have been used, and as a result, as the molecular weight increases, the emulsifying power decreases, In some cases, it has become impossible to produce a uniform O/Wl emulsion using this method.

このよつな傾向(乳化力の減衰)を示す非イオン界面活
性剤としては、例えば硬化ヒマシ油ポリエチレンオキシ
ド付加物、シ璽糖脂肪酸エステル、ポリ(オキシプロピ
レンコポリ(オキシエチレン)アルキルエーテルなどが
挙げられる。
Examples of nonionic surfactants that exhibit this tendency (attenuation of emulsifying power) include hydrogenated castor oil polyethylene oxide adducts, silica fatty acid esters, and poly(oxypropylene copoly(oxyethylene) alkyl ethers). It will be done.

ま九、これまでの方法では、分子量の論議を別にしても
乳化剤と油の種類との組合せ例えばポリオキシエチレン
脂肪酸エステルとトリグリセライド油の場合に見られる
如く、均一なO/W型エマルジョンが得られないことも
あった。
9. In the conventional methods, apart from the discussion of molecular weight, it is difficult to obtain a uniform O/W emulsion due to the combination of emulsifier and oil type, for example, as seen in the case of polyoxyethylene fatty acid ester and triglyceride oil. Sometimes I couldn't.

そこで、本発明者は、前記の如き乳化力が弱く均一なエ
マルジ冒ンの調製が困難な乳化剤を用いた場合でも、均
−且つ安定なエマルジ冒ンを得る方法を見い出さんと種
々実験研究を繰返した結果、本発明の完成に至ったもの
である。
Therefore, the present inventor conducted various experimental studies to find a method for obtaining a uniform and stable emulsion even when using an emulsifier with weak emulsifying power and difficulty in preparing a uniform emulsion as described above. As a result of repeated efforts, the present invention was completed.

すなわち、本発明は、まず第1工程として界面活性剤と
油相とを、場合により加熱しながら分散乃至は溶解混合
し、次いでこれに分子中に水酸基を2個以上有する水溶
性多価アルコールと水との混合溶液を少量ずつ添加して
ゲル状もしくは透明液状組成物を形成し、第2工程とし
て第1工程で得られたゲル状もしくは透明液状組成物と
水相とを混合して希釈することを特徴とする水中油型エ
マルジ謬ンの製造方法に関するものである。
That is, in the present invention, as a first step, a surfactant and an oil phase are dispersed or dissolved and mixed, optionally with heating, and then a water-soluble polyhydric alcohol having two or more hydroxyl groups in the molecule is added to the mixture. A mixed solution with water is added little by little to form a gel-like or transparent liquid composition, and in a second step, the gel-like or transparent liquid composition obtained in the first step is mixed with an aqueous phase to dilute it. The present invention relates to a method for producing an oil-in-water emulsion characterized by the following.

以下、本発明の詳細な説明する。The present invention will be explained in detail below.

本発明に適用される界面活性剤としては、一般的に乳化
に使用されるものは全て用いることができる。また、H
LB的には必ずしも制約を受けないが、よシ親水的なも
のが好ましい。具体的には、例えばソルビタン脂肪酸エ
ステル、グリセリン脂肪酸エステル、ポリグリセリン脂
肪酸エステル、プロピレングリコール脂肪酸エステル、
ポリオキシエチレンソルビタン脂肪酸エステル、ポリオ
キシエチレンソルビタン脂肪酸エステル、グリセリン脂
肪酸エステルのポリエチレンオキシド付加物ポリオキシ
エチレン脂肪酸エステル、ポリオキシエチレンアルキル
エーテル、ポリ(オキシエチレン) ホIJ (オキシ
プロピレン)アルキルエーテル、ポリグロピレングリコ
ールポリエチレンオキシド付加物、硬化ヒマシ油ポリエ
チレンオキシド付加物、シ璽塘脂肪酸−エステル、ポリ
オキシエチレンコレステロールエーテルなどの非イオン
性界面活性剤を中心として、その他アシル化ベプタイド
などが挙げられるが、中でも前述の如く通常の乳化法で
は継子を形成したり、油分数のできない水−活性剤ゲル
を形成したりして良好なエマルジ冒ンを調製し難い硬化
ヒマシ油ポリエチレンオキシド付加物、ポリ(オキシエ
チレン)ポリ(オキシプロピレン)アルキルエーテル、
シ房糖脂肪酸zステルなどが好適である。
As the surfactant applicable to the present invention, all those commonly used for emulsification can be used. Also, H
Although not necessarily limited in terms of LB, highly hydrophilic ones are preferred. Specifically, for example, sorbitan fatty acid ester, glycerin fatty acid ester, polyglycerin fatty acid ester, propylene glycol fatty acid ester,
Polyoxyethylene sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, polyethylene oxide adduct of glycerin fatty acid ester polyoxyethylene fatty acid ester, polyoxyethylene alkyl ether, poly(oxyethylene) (oxypropylene) alkyl ether, polyglot Mainly non-ionic surfactants such as pyrene glycol polyethylene oxide adducts, hydrogenated castor oil polyethylene oxide adducts, silicate fatty acid esters, and polyoxyethylene cholesterol ethers, as well as other acylated peptides, among others. As mentioned above, hydrogenated castor oil polyethylene oxide adducts, poly(oxyethylene ) poly(oxypropylene) alkyl ether,
Suitable examples include cephalic sugar fatty acid z stel.

次に、油相もfFK限定されず、オリーブ油、大豆油、
牛脂等の動植物油脂、ミツロウ、カルナウバロウ、ラノ
リン等のロウ類、パラフィン、マイクロクリスタリンワ
ックス等の炭化水素類、パルミチン酸、オレイン酸等の
高級脂肪酸類、セタノール、コレステロール等の高級ア
ル:F−ル類、 イングロビルミリステート、2−エチ
ルヘキサン酸セチル、ミリスチン酸オクチルドデシル等
のエステル類、その他シリコーン油など幅広いものが適
用可能である。
Next, the oil phase is not limited to fFK, but includes olive oil, soybean oil,
Animal and vegetable oils and fats such as beef tallow, waxes such as beeswax, carnauba wax, and lanolin, hydrocarbons such as paraffin and microcrystalline wax, higher fatty acids such as palmitic acid and oleic acid, and higher alcohols such as cetanol and cholesterol. A wide range of esters such as , inglovir myristate, cetyl 2-ethylhexanoate, octyldodecyl myristate, and other silicone oils can be used.

ここで、界面活性剤と油相との混合に際し、界面活性剤
は油相量に対して7重t%以上好ましくはlO!量チ以
上が添加される。7重11%より少なくなるとエマルジ
四ノの安定性が低下して好ましくないが、上限について
は特に制約はない。
Here, when mixing the surfactant and the oil phase, the surfactant should preferably be 7% by weight or more of 1O! based on the amount of the oil phase. More than 50% of the amount is added. If it is less than 11% by weight, the stability of the emulsion will decrease, which is not preferable, but there is no particular restriction on the upper limit.

また、混合温度については、均一分散乃至は溶解が為さ
れるならば常湿でも構わないが、固体脂を用いた場合、
または均一分散乃至は溶解を促進するため、場合により
加熱(約85℃位まで〕下で混合すると効果的である。
Regarding the mixing temperature, normal humidity may be used as long as uniform dispersion or dissolution is achieved, but if solid fat is used,
Alternatively, in order to promote uniform dispersion or dissolution, it may be effective to mix under heating (up to about 85° C.) as the case may be.

次に1水溶性多価アルコールとしては、その分子中に2
個以上の水酸基を有するもので、例えばエチレングリコ
ール、フロピレンゲリコール、l、3−ブタンジオール
、l、4−7’タンジオール、1.5−ベンタンジオー
ル、ポリエチレンクリコール(200,400,600
,1000,1500人グリセリン、ジグリセリン、ト
リグリセリン、ポリグリセリン、シ璽糖、グルコース、
麦芽糖などが用いられる。そして、水溶性多価アルコー
ルと水とは重量比で882〜2:8、好ましくは7:3
〜3ニアの範囲で混合されたものが第1工程で使用され
る。多価液状組成物を形成せず、これを水相と混合して
も均一なO/Wfiエマルジ四ンとはなり得ない。逆に
水の比率が前記範囲より大きくなると、例えば分子量が
2000以上の非イオン界面活性剤を主成分とする乳化
剤を用いた時にゲル状もしくは透明液状組成物を形成せ
ず、これを水相と混合しても均一なO/Wfflエマル
ジ璽ンとならない。
Next, as a 1 water-soluble polyhydric alcohol, there are 2 in its molecule.
Polyethylene glycol (200,400,600
, 1000, 1500 people Glycerin, diglycerin, triglycerin, polyglycerin, sucrose, glucose,
Maltose etc. are used. The weight ratio of water-soluble polyhydric alcohol and water is 882 to 2:8, preferably 7:3.
A mixture in the range of ~3Nia is used in the first step. Even if a multivalent liquid composition is not formed and mixed with an aqueous phase, a uniform O/Wfi emulsion cannot be obtained. On the other hand, if the ratio of water is larger than the above range, for example, when using an emulsifier whose main component is a nonionic surfactant with a molecular weight of 2,000 or more, a gel-like or transparent liquid composition will not be formed, and this will not form a water phase. Mixing does not result in a uniform O/Wffl emulsion.

また、第1工程で油相に徐々に添加される上記水溶性多
価アルコールと水との混合溶液の添加量は、界面活性剤
を含む全油相lに対して0.1重量倍以上、好ましくは
0.2重量倍以上で且つ上限は2重量倍以下でなければ
ならない。0.1重量倍より少ない添加量では、油連続
相がゲル状もしくは透明液状均一相にならないため、こ
れを水相と混合しても均一な安定エマルジ冒ンが得られ
ない。
Further, the amount of the mixed solution of water-soluble polyhydric alcohol and water that is gradually added to the oil phase in the first step is 0.1 times or more by weight based on the total oil phase 1 containing the surfactant, It is preferably 0.2 times by weight or more, and the upper limit must be 2 times by weight or less. If the amount added is less than 0.1 times by weight, the oil continuous phase will not become a gel-like or transparent liquid homogeneous phase, and even if it is mixed with the aqueous phase, a uniform stable emulsion cannot be obtained.

反対に、2重量倍を越える添加量では、そのまま乃至は
水相との混合後に一応0/W型エマルジ璽ンとはなるが
、合一安定性が悪く、良好なエマルジ曹ンを得ることは
できない。
On the other hand, if the amount added exceeds 2 times the weight, a 0/W type emulsion can be obtained as it is or after mixing with an aqueous phase, but the coalescence stability is poor and it is difficult to obtain a good emulsion. Can not.

斯る如くして得られたゲル状もしくは透明液状組成物は
、第2工程で水相と混合される。混合に際しては、ゲル
状もしくは透明液状組成物を水相で希釈しても良いし、
またはゲル状もしくは透明液状組成物を水相へ分散させ
ても良く、何れの方法でも可能である。
The gel-like or transparent liquid composition thus obtained is mixed with an aqueous phase in a second step. When mixing, the gel or transparent liquid composition may be diluted with an aqueous phase, or
Alternatively, a gel or transparent liquid composition may be dispersed in an aqueous phase, and any method is possible.

また□、ゲル状もしくは透明液状組成物と水相との混合
比率は、0.01〜99.9:99.9〜01O1の範
囲で任意に変動させ得るが、エマルジ四ンの安定性を考
慮した場合にはゲル状もしくは透明液状組成物に対して
300重量以上の水相を混合することが有利である。
□The mixing ratio of the gel-like or transparent liquid composition and the aqueous phase can be arbitrarily varied within the range of 0.01-99.9:99.9-01O1, but the stability of the emulsion is taken into consideration. In such cases, it is advantageous to mix 300 weight or more of the aqueous phase with respect to the gel or transparent liquid composition.

ここで、本発明の方法の特徴について述べると、これま
で油への分散性が悪く、ま九は乳化力が弱く乳化剤とし
ての利用が困難であったポリ(オキシエチレン)ポリ(
オキシプロピレン)アルキルエーテル、硬化ヒマシ油ポ
リエチレンオキシド付加物ならびにショ糖脂肪酸エステ
ルなどを用いた場合にも、有効な乳化力を発揮させ得る
様にしたことである。すなわち、第1工程における多価
アルコール水溶液の添加により、界面活性剤の油への分
散乃至は溶解性が向上し、透明な油溶液となり、さらに
添加が進むと液晶組成分を形成する様になる。更に添加
が進むと、多価アルコール水溶液中に油が可溶化された
透明溶液となる。これは多価アルコール成分が分子会合
力を弱め、分散性を向上させる働きがあるためと考察さ
れる。しかし、多価アルコールのみを添加した場合には
、界面活性剤は分子会合体を形成できず、第1工程終了
時にゲル状もしくは透明液状組成物を形成できない。従
って、安定なエマルジョンも得られなくなりてしまう。
Here, to describe the characteristics of the method of the present invention, poly(oxyethylene) poly(oxyethylene), which has until now had poor dispersibility in oil and weak emulsifying power, has been difficult to use as an emulsifier.
This makes it possible to exhibit effective emulsifying power even when using oxypropylene) alkyl ether, hydrogenated castor oil polyethylene oxide adduct, sucrose fatty acid ester, etc. That is, the addition of the polyhydric alcohol aqueous solution in the first step improves the dispersion or solubility of the surfactant in oil, resulting in a transparent oil solution, and as the addition progresses further, a liquid crystal component is formed. . As the addition progresses further, a transparent solution in which the oil is solubilized in the aqueous polyhydric alcohol solution is formed. This is considered to be because the polyhydric alcohol component weakens the molecular association force and improves dispersibility. However, when only a polyhydric alcohol is added, the surfactant cannot form a molecular association, and a gel-like or transparent liquid composition cannot be formed at the end of the first step. Therefore, it becomes impossible to obtain a stable emulsion.

熱論、本発明の方法は、従来法でも通常の乳化力を有し
ているポリオキシエチレンンルビタン脂肪酸エステル、
ポリオキシエチレンアルキルエーテル、またはポリオキ
シエチレン脂肪酸エステルなどの乳化剤を用いる場合で
も適用される。斯る場合には、従来法を用いる場合より
も乳化剤の使用量を減少させ得る有利さがある。
Thermal theory, the method of the present invention uses polyoxyethylene rubitan fatty acid ester, which has normal emulsifying power even in conventional methods.
It is also applicable when using an emulsifier such as polyoxyethylene alkyl ether or polyoxyethylene fatty acid ester. In such a case, there is an advantage that the amount of emulsifier used can be reduced compared to when using conventional methods.

尚、最近ではエマルジ冒ン調製時に多価アルコールを利
用する技術が幾つか開示されているが、何れも乳化剤と
多価アルコールもしくは多価アルコール水溶液とを先ず
混合溶解したものに油相を添加してゆく方法であり、そ
の作用機序からして本発明の方法とは全く異なるもので
ある。
Recently, several techniques have been disclosed that use polyhydric alcohols when preparing emulsions, but in all of them, an oil phase is added to a mixture of an emulsifier and a polyhydric alcohol or an aqueous solution of a polyhydric alcohol. This method is completely different from the method of the present invention in terms of its mechanism of action.

この様に1本発明の方法は従来法にない高い有用性をも
つものであり、この方法を用いることKよってより安全
で安定性の高い医薬品、化粧品、食品などを提供するこ
とができる。
As described above, the method of the present invention is highly useful compared to conventional methods, and by using this method, safer and more stable pharmaceuticals, cosmetics, foods, etc. can be provided.

次に1本発明の方法の重要な要素である第1工程で添加
される多価アルコール水溶液において、多価アルコール
と水との混合比が如何に工iルジ璽ン調製に影響を及ぼ
すかを示すため行なりた実験例を以下に示す。方法とし
ては、下記の乳化系組成中における水溶性多価アルコー
ル(プロピレングリコール)と水の比率を順次変えてゆ
き、本発明の方法に従って調製されたエマルジ曹ンの状
態を評価して、その結果を表−1に示した。
Next, we will examine how the mixing ratio of polyhydric alcohol and water in the polyhydric alcohol aqueous solution added in the first step, which is an important element of the method of the present invention, affects the preparation of alcoholic beverages. An example of an experiment conducted to demonstrate this is shown below. The method involved sequentially changing the ratio of water-soluble polyhydric alcohol (propylene glycol) and water in the emulsion system composition below, and evaluating the state of the emulsion carbon prepared according to the method of the present invention. are shown in Table-1.

く乳化系組成〉         (重量部)POE(
34)POP(23)ステアリルエーテル  5流動パ
ラフイン           20プロピレングリー
−ル(PG)      X精  製  水     
               10− X精 製 水
(希釈用)65 く評価基準〉 0: 均一なO/W型エマルジ曹ン Δ:  不均一なo/W凰エマルシ肩ン×: 乳化され
ない 表−1 表−1の結果にも示されたように、水溶性多価アルコー
ルの混合比率が20重量−以下でも、また80重量%以
上でも均一なo7wをエマルジ1/が得られないことが
明らかとなった。
Emulsifying system composition> (parts by weight) POE (
34) POP (23) Stearyl ether 5 Liquid paraffin 20 Propylene glycol (PG) X Purified water
10-X Purified water (for dilution) 65 Evaluation criteria> 0: Uniform O/W type emulsion Δ: Non-uniform O/W type emulsion ×: Not emulsified Table-1 Results of Table-1 As shown in the above, it became clear that even if the mixing ratio of the water-soluble polyhydric alcohol was less than 20% by weight or more than 80% by weight, a uniform o7w emulsion 1/1 could not be obtained.

更に、本発明の方法が如何に均一なO/W型エマルジ璽
ンを与え得るかを示すため、後記実施例IK示した本発
明の方法によるO/W型エマルジョンと化粧品として後
記比較例1及び2に示した従来法(反転乳化法)Kよる
乳化物及びこれを更にホモミキサー処理して得られたO
/Wfiエマルジ曹ンとを用いて、エマルジW/の粒度
分布状態を測定した。測定方法としては、遠心式自動粒
度分布測定装置CAPA500(堀場製作所製)を用い
、その結果を第1図(実施例1)及び第2図(比較例2
)K示した。尚、比較例1の乳化物については全<0/
Wをエマルジョン状態とはなりていなかり九。
Furthermore, in order to show how the method of the present invention can give a uniform O/W emulsion, the O/W emulsion according to the method of the present invention shown in Example IK below and Comparative Example 1 and Comparative Example 1 below as cosmetics were prepared. Emulsion obtained by the conventional method (inversion emulsification method) K shown in 2 and O obtained by further treating this with a homomixer
/Wfi emulsion carbonate was used to measure the particle size distribution of emulsion W/. As a measurement method, a centrifugal automatic particle size distribution analyzer CAPA500 (manufactured by Horiba, Ltd.) was used, and the results are shown in Figure 1 (Example 1) and Figure 2 (Comparative Example 2).
) K was shown. In addition, for the emulsion of Comparative Example 1, total <0/
W is not in an emulsion state.9.

第1図及び第2図の結果に示された如く、本発明の方法
(実施例1)によるO/W′mエマルジ冒ンは平均粒度
が1.1μm と小さく、しかも分布が狭く均一性が高
いのに対し、従来法(比較例2)Kよる0/WW工iル
ジ鵞ンは平均粒度が2.4μmと大きく、しかも分布が
広いといり状態が明らかとなり、本発明の方法の優秀性
が証明された。
As shown in the results in Figures 1 and 2, the O/W'm emulsion obtained by the method of the present invention (Example 1) has a small average particle size of 1.1 μm, and has a narrow distribution and uniformity. On the other hand, the conventional method (comparative example 2) K-based 0/WW milled grain had a large average particle size of 2.4 μm, and the distribution was wide, making it clear that the cracked state was excellent, demonstrating the superiority of the method of the present invention. has been proven.

以下に、本発明の方法の実施例及び比較例を示すO 実施例1 POE(6’0)硬化ヒマシ油29、ソルビタンモノス
テアレート22、流動パラフィン20.9を200 m
l  ビーカーに採り、80℃の水浴上で混合溶解した
。この溶液に攪拌しながらプロピレングリコール49、
水4IIの混合溶液を80℃に加熱した後、徐々に添加
してゲル状組成物を得た。
Examples and comparative examples of the method of the present invention are shown below.
The mixture was placed in a beaker and mixed and dissolved on a water bath at 80°C. Add propylene glycol 49 to this solution while stirring.
A mixed solution of water 4II was heated to 80° C. and then added gradually to obtain a gel composition.

次にこれに水68.9を加えて希釈し、その後冷却して
O/W型エマルジ曹ン1ooIiを得た。
Next, this was diluted by adding 68.9 g of water, and then cooled to obtain O/W type emulsion carbon 1ooIi.

比較例1 POI(60)[化ヒマシ油2.9.ソルビタンモノス
テアレート2.9.流動パラフィン20.9を200 
ml  ビーカーに採り、80℃の水浴上で混合溶解し
た。別に、プロピレングリコール4gと水7219の混
合溶液を80℃に加熱し九後、油相中に水相を徐々に加
えてゆき、反転乳化を行なりた。これを、更に攪拌しな
がら冷却し、乳化物100Nを得た。
Comparative Example 1 POI (60) [Converted castor oil 2.9. Sorbitan monostearate 2.9. Liquid paraffin 20.9 to 200
ml beaker and mixed and dissolved on a water bath at 80°C. Separately, a mixed solution of 4 g of propylene glycol and 7,219 g of water was heated to 80° C., and then the aqueous phase was gradually added to the oil phase to perform inversion emulsification. This was further cooled while stirring to obtain a 100N emulsion.

比較例2 比較例1で得られた乳化物を、ホモミキサーで8000
rpm、4分間処理した後、冷却して釦W型エマルジョ
ン100gを得た。
Comparative Example 2 The emulsion obtained in Comparative Example 1 was heated to 8,000 ml using a homomixer.
rpm for 4 minutes, and then cooled to obtain 100 g of a button W-shaped emulsion.

実施例2 POE(30)POP(25)オレイルエーテル5II
、セメノール3Ii、ステアリン酸3g、オリープ油1
0 g、流動パラフィン20.Fを70℃で混合した。
Example 2 POE (30) POP (25) Oleyl Ether 5II
, Semenol 3Ii, stearic acid 3g, olive oil 1
0 g, liquid paraffin 20. F was mixed at 70°C.

これにグリセリン411.水611の混合溶液を70℃
に加熱した後、徐々に攪拌しながら加えてゲル状組成物
を形成させた。次に水49Iiを70℃に加熱し、これ
をゲル状組成物に徐々に加え、充分攪拌を行なった後、
冷却してO/WWエマルジ璽ン100#を得た。
Add this to glycerin 411. A mixed solution of 611 water at 70℃
and then gradually added with stirring to form a gel-like composition. Next, water 49Ii was heated to 70°C, and this was gradually added to the gel composition, and after thorough stirring,
It was cooled to obtain O/WW emulsion bottle 100#.

実施例3 シ璽糖モノステアレート4I、セタノールlI。Example 3 Citrus sugar monostearate 4I, cetanol lI.

大豆油30.9を70℃で混合した。これにプロピレン
グリコール319.水711の混合溶液を70℃とし、
徐々に添加攪拌してゲル状組成物とした。
30.9 g of soybean oil was mixed at 70°C. This is propylene glycol 319. A mixed solution of water 711 was heated to 70°C,
The mixture was gradually added and stirred to form a gel-like composition.

次に水55gを70℃に加熱して、ゲル状組成物にゆっ
くりと加えて充分攪拌を行なった後、冷却してO/W型
エマルジ冒ン100,9を得た。
Next, 55 g of water was heated to 70° C., slowly added to the gel composition, thoroughly stirred, and then cooled to obtain O/W emulsion 100.9.

実施例4 POE(20)ソルビタンモノステアレート3.9.P
OE(50)硬化ヒマシ油lI、セタノール4N、ステ
アリン@21.グリセリルトリー2−エチルヘキシルエ
ーテル25 Iiミラ 0℃テ混合溶解した。これに、
ポリエチレングリコール(600)611.水sIIの
混合溶液を80℃に加熱したものを、添加攪拌してゲル
状組成物を得た。次に、これをアミノ酸、水溶性香料、
保湿剤を含んだ水相549で希釈し、更に25℃まで冷
却して0/W凰エマルジ璽ン(クリーム)loO,Pを
得た。
Example 4 POE(20) Sorbitan Monostearate 3.9. P
OE (50) Hydrogenated castor oil lI, Setanol 4N, Stearin@21. Glyceryl tri-2-ethylhexyl ether 25 Ii Mira was mixed and dissolved at 0°C. to this,
Polyethylene glycol (600) 611. A mixed solution of water sII heated to 80° C. was added and stirred to obtain a gel composition. Next, this is combined with amino acids, water-soluble fragrance,
The mixture was diluted with an aqueous phase 549 containing a humectant and further cooled to 25° C. to obtain 0/W emulsion (cream) loO,P.

【図面の簡単な説明】[Brief explanation of the drawing]

第1図は実施例1で得られたO/W型エマルジョンの粒
度(μmrL)と分布度(情の結果を示したものである
。第2図は比較例2で得られたO/WWエマルジ曹ンの
粒度(μIm)と分布度(情の結果を示したものである
。 特許出願人 ポーラ化成工業株式会社 第1図 分布度 (%) 第2図 分布度 (%)
Figure 1 shows the particle size (μmrL) and distribution degree (information) of the O/W emulsion obtained in Example 1. Figure 2 shows the results of the O/W emulsion obtained in Comparative Example 2. This shows the results of particle size (μIm) and distribution (%) of carbon. Patent applicant: POLA CHEMICAL INDUSTRIES, INC. Figure 1 Distribution (%) Figure 2 Distribution (%)

Claims (1)

【特許請求の範囲】 1)第1工程として界面活性剤と油相とを混合し、次い
でこれに水溶性多価アルコールと水との混合溶液を添加
してゲル状もしくは透明液状組成物を形成し、第2工程
として該ゲル状もしくは透明液状組成物と水相とを混合
することを特徴とする水中油型エマルジョンの製造方法
。 2)界面活性剤の混合量が油相量に対して7重量%以上
である特許請求の範囲第1)項記載の水中油型エマルジ
ョンの製造方法。 3)水溶性多価アルコールと水との混合重量比が8:2
から2:8の範囲である特許請求の範囲第1)項記載の
水中油型エマルジョンの製造方法。 4)水溶性多価アルコールと水との混合溶液の添加量が
界面活性剤を含む全油相量に対して0.1〜2倍量の範
囲である特許請求の範囲第1)項記載の水中油型エマル
ジョンの製造方法。
[Claims] 1) As a first step, a surfactant and an oil phase are mixed, and then a mixed solution of a water-soluble polyhydric alcohol and water is added to form a gel-like or transparent liquid composition. A method for producing an oil-in-water emulsion, which comprises mixing the gel or transparent liquid composition with an aqueous phase as a second step. 2) The method for producing an oil-in-water emulsion according to claim 1), wherein the amount of the surfactant mixed is 7% by weight or more based on the amount of the oil phase. 3) The mixing weight ratio of water-soluble polyhydric alcohol and water is 8:2
A method for producing an oil-in-water emulsion according to claim 1, wherein the ratio is from 4) Claim 1), wherein the amount of the mixed solution of water-soluble polyhydric alcohol and water added is in the range of 0.1 to 2 times the amount of the total oil phase containing the surfactant. Method for producing oil-in-water emulsions.
JP61252455A 1986-10-23 1986-10-23 Preparation of oil-in-water-type emulsion Pending JPS63107740A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP61252455A JPS63107740A (en) 1986-10-23 1986-10-23 Preparation of oil-in-water-type emulsion

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP61252455A JPS63107740A (en) 1986-10-23 1986-10-23 Preparation of oil-in-water-type emulsion

Publications (1)

Publication Number Publication Date
JPS63107740A true JPS63107740A (en) 1988-05-12

Family

ID=17237617

Family Applications (1)

Application Number Title Priority Date Filing Date
JP61252455A Pending JPS63107740A (en) 1986-10-23 1986-10-23 Preparation of oil-in-water-type emulsion

Country Status (1)

Country Link
JP (1) JPS63107740A (en)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6140375A (en) * 1996-05-23 2000-10-31 Taisho Pharmaceutical Co., Ltd. Microemulsion
JP2005104884A (en) * 2003-09-30 2005-04-21 Nof Corp Skin cosmetic
JP2005193134A (en) * 2004-01-06 2005-07-21 Shiseido Co Ltd One-phase microemulsion composition and its manufacturing method
JP2005194229A (en) * 2004-01-06 2005-07-21 Shiseido Co Ltd O/w ultrafine emulsion preparation for external use and method for producing the same
JP2007063197A (en) * 2005-08-31 2007-03-15 Hoyu Co Ltd Hair cosmetic
US8461214B2 (en) 2004-01-06 2013-06-11 Shiseido Co., Ltd. One-phase microemulsion compositions, O/W ultrafine emulsion external formulations and method for producing the same
JP2015510441A (en) * 2011-11-29 2015-04-09 アート−エフアイ Compositions that mimic the dielectric properties of the human body and their use for SAR measurements

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6140375A (en) * 1996-05-23 2000-10-31 Taisho Pharmaceutical Co., Ltd. Microemulsion
JP2005104884A (en) * 2003-09-30 2005-04-21 Nof Corp Skin cosmetic
JP4529402B2 (en) * 2003-09-30 2010-08-25 日油株式会社 Skin cosmetics
JP2005193134A (en) * 2004-01-06 2005-07-21 Shiseido Co Ltd One-phase microemulsion composition and its manufacturing method
JP2005194229A (en) * 2004-01-06 2005-07-21 Shiseido Co Ltd O/w ultrafine emulsion preparation for external use and method for producing the same
US8461214B2 (en) 2004-01-06 2013-06-11 Shiseido Co., Ltd. One-phase microemulsion compositions, O/W ultrafine emulsion external formulations and method for producing the same
JP2007063197A (en) * 2005-08-31 2007-03-15 Hoyu Co Ltd Hair cosmetic
JP2015510441A (en) * 2011-11-29 2015-04-09 アート−エフアイ Compositions that mimic the dielectric properties of the human body and their use for SAR measurements
US9709615B2 (en) 2011-11-29 2017-07-18 Art-Fi Composition simulating the dielectric properties of the human body and use thereof for SAR measurement

Similar Documents

Publication Publication Date Title
EP0174377B1 (en) W/o/w complex emulsion for medicinal or cosmetic use
US5976604A (en) Oil-in-water emulsion composition having high oil content and method for producing the same
JPS6361050B2 (en)
JP2008511550A (en) Process for producing microemulsion and submicron emulsion and composition
JP4963958B2 (en) Stable concentrated and diluted oil-in-water emulsions, processes for their preparation, and formulation processes using these emulsions
JPH1190211A (en) Preparation of o/w type emulsion
JPH05279248A (en) Production and cosmetic use of stable combination emulsion system of water-oil-water type
JPS63107740A (en) Preparation of oil-in-water-type emulsion
JP4048342B2 (en) W / O type emulsion composition and method for producing the same
JPH08283303A (en) Emulsifier comprising higher fatty acid dextrin, emulsion composition containing the same, and cosmetic
JPS61129033A (en) Water in oil emulsifier composition
JP3639715B2 (en) Finely dispersed composition of wax, hair cosmetic and polish
JPS641173B2 (en)
JPS60193529A (en) Production of w/o/w type emulsion
JPH0559890B2 (en)
JP3424770B2 (en) Water-in-oil emulsion composition
JP2001048742A (en) Cosmetic
JP2535902B2 (en) Method for producing oil-in-water emulsion
JPH1118697A (en) Oil-containing gel-like composition and oil-in-water type emulsified composition
JPS63143935A (en) Manufacturing of emulsion
JPS63126541A (en) Low-water content o/w type emulsion and its production
JPH0720543B2 (en) Method for producing gel emulsion and oil-in-water emulsion
JP3779824B2 (en) High internal water phase emulsion composition
JPH11158032A (en) High-inner-aqueous phase emulsion composition
JP3752767B2 (en) High oil content oil-in-water emulsified composition and method for producing the same