JPS5946123A - Preparation of gel like emulsion and oil in water type emulsion - Google Patents

Preparation of gel like emulsion and oil in water type emulsion

Info

Publication number
JPS5946123A
JPS5946123A JP15438182A JP15438182A JPS5946123A JP S5946123 A JPS5946123 A JP S5946123A JP 15438182 A JP15438182 A JP 15438182A JP 15438182 A JP15438182 A JP 15438182A JP S5946123 A JPS5946123 A JP S5946123A
Authority
JP
Japan
Prior art keywords
oil
water
emulsion
gel
surfactant
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.)
Granted
Application number
JP15438182A
Other languages
Japanese (ja)
Other versions
JPH0251665B2 (en
Inventor
Yoshie Muramatsu
村松 宜江
Sadao Hoshizaki
星崎 貞夫
Shinya Okabe
慎也 岡部
Yoshikazu Hirai
義和 平井
Kazuo Nabeta
鍋田 一男
Hiromichi Sagiya
鷺谷 広道
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 JP15438182A priority Critical patent/JPS5946123A/en
Publication of JPS5946123A publication Critical patent/JPS5946123A/en
Publication of JPH0251665B2 publication Critical patent/JPH0251665B2/ja
Granted 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
    • A61K8/042Gels
    • 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
    • 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

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Veterinary Medicine (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Birds (AREA)
  • Epidemiology (AREA)
  • Dermatology (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Cosmetics (AREA)
  • Colloid Chemistry (AREA)

Abstract

PURPOSE:To prepare an oil-in-surfactant type gel like emulsion, by gradually adding an oil phase component to a surfactant continuous phase having an aqueous phase component consisting of a water soluble solvent and water and a nonionic surfactant dissolved therein. CONSTITUTION:An aqueous phase component wherein a water soluble solvent selected from one kind of more glycols or a derivative thereof (e.g., propylene glycol) and water are within a range of 3:7-8:2 and a nonionic surfactant (e.g., sorbitan fatty acid ester) are dissolved to prepare a surfactant continuous phase. In the next step, an oil phase component (e.g., squalane) is gradually added to prepare an oil in surfactant type gel like emulsion. Because thus obtained gel like emulsion is resistant to agglomeration, it is hardly restricted by various conditions during a production process and a stable O/W emulsion can be easily prepared and, at the same time, the gel like emulsion itself can be utilized as a product.

Description

【発明の詳細な説明】 本発明は新規なゲル状エマル7ヨノ及O・水中油型エマ
ルションの製造法に関するものである1、更に詳しく述
べると、水溶性溶媒と水からなる水相成分と非イオン界
面活性剤とを溶解させだ界「■1活性剤連続相に対し、
油相成分を徐々に冷力1]ぜしめて界面活性剤中油より
なるケル状エマルンヨンを得る製造法、及び該エマルシ
ョンに水相を添加することによって?T)られるη定な
水中油型エマルションの製造法にロー1するものである
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing a novel gel-like emulsion and an oil-in-water emulsion. When the ionic surfactant is dissolved,
1] A manufacturing method for obtaining a gel-like emulsion consisting of oil in a surfactant by gradually cooling the oil phase components, and by adding an aqueous phase to the emulsion? T) This is a method for producing an oil-in-water emulsion with a constant η.

一般に、これまで行われている界面活性剤の添加方法と
しては、予め界面活性剤を油相中に添加しておく所謂エ
ージェントインオイル(a、gent in oil 
)法や、逆に水相中にW iM’i li’+性剤を添
加しておくニージエントイノウオー−ター(agent
 in va、ter )法、さらには731水件界自
活性剤を水相に親油性界面活性剤を油相中に溶解してお
く方法がある。従来、ゲル状エマルションハ、前記エー
ジェントインオイルの製造過程における転相直後の重粘
な状態を利用したり、ペースト法すなわち少量の水相に
乳化剤を加えこれに油相を少量づつ加えて行く方法によ
って製造されていたが、転相法、ペー、スト法共に使用
するIIL13の調節が極めて難しいとされている。
Generally, the conventional method of adding surfactants is the so-called agent-in-oil method, in which a surfactant is added into the oil phase in advance.
) method, or conversely, the nee- ient inno water (agent
There is a method in which a 731 water-based surfactant is dissolved in an aqueous phase and a lipophilic surfactant is dissolved in an oil phase. Conventionally, gel emulsions have been used, such as by utilizing the heavy viscous state immediately after the phase inversion in the agent-in-oil manufacturing process, or by using the paste method, in which an emulsifier is added to a small amount of the aqueous phase and the oil phase is added little by little. However, it is said that it is extremely difficult to adjust IIL13, which is used for both the phase inversion method and the paste method.

例えば、前者の転相法においては、親油側に傾いている
と水を添加しても反転しないのでゲル状エマルンヨンは
得られない。逆に親水側に11LBが傾いていた場合に
は、ゲルエマルションに油相が分散せず、反転後たソち
に分離してしまう状態を呈する。後者のペースト法にお
いては、親油側の場合、界面活性剤の水への分散性が悪
く油相を加えてもエマル/ヨン状態にはならず、単なる
分離系を呈するにすぎない。逆に親水側では水相に界面
活性剤が完全に溶解してしまい、油相を添加したときに
油滴が大きくて瞬時にて合一、分離してし1う傾向があ
る。
For example, in the former phase inversion method, if it is tilted toward the lipophilic side, it will not be reversed even when water is added, and a gel-like emulsion cannot be obtained. On the other hand, if 11LB is tilted toward the hydrophilic side, the oil phase will not be dispersed in the gel emulsion and will separate immediately after inversion. In the latter paste method, in the case of the lipophilic side, the dispersibility of the surfactant in water is poor, and even if an oil phase is added, an emulsion/yellow state is not obtained, but a mere separation system is formed. On the other hand, on the hydrophilic side, the surfactant is completely dissolved in the water phase, and when the oil phase is added, the oil droplets are large and tend to coalesce and separate instantly.

これらの背景から、安定なゲル状エマルンヨンの製造法
として、界面活性剤J)親水性−現油性バランス(HL
B )を厳密に調整し、界面活性剤を予め油相へ溶解し
ておくことが大切であると指摘されている。そして、乳
化剤の選定にあたっては、グリフインによって確立され
たIILIi値の概念が利用されている。この概念によ
る払ゲル状エマルンヨンを製造するのに適したIll□
13値は8〜]3の範囲とされているが、実際に安定な
エマルションを得るには油の種類や配合(11:によっ
てかなり精度のよいHLB値の調整が心安てあった。さ
らに、これまで提供されているゲル状エマルション製品
は共通して耐温性が比較的悪く、例えば40’〜45℃
の過酷条件では生成ゲ/l/がこわれて流動性を呈する
傾向にあった。
From these backgrounds, as a method for producing stable gel-like emulsion, surfactant J) hydrophilic-oleaginous balance (HL
It has been pointed out that it is important to strictly adjust B) and to dissolve the surfactant in the oil phase in advance. In selecting an emulsifier, the concept of IILIi value established by Griffin is utilized. Ill□ suitable for producing gel-like emulsion based on this concept
The 13 value is said to be in the range of 8 to] 3, but in order to actually obtain a stable emulsion, it is safe to adjust the HLB value with high accuracy depending on the type and composition of oil (11:).Furthermore, this Gel-like emulsion products offered up to
Under such severe conditions, the resulting product /l/ tended to break down and exhibit fluidity.

一方、安定な水中油型エマルションをイ1)る製造法と
しては、今日まででは、上記したエージェントインオイ
ル法が優れていると報告されている。このエージェント
インオイル法は、非イオン界面活性剤を油相に溶解さぜ
、次にこの油相に水相を添加し転相によって水中油型エ
マル7ョンを得る方法であるが、実際の水中油型の製造
においては、前述のゲル状エマル/ヨノの問題を含め、
本方法を用いてもいくつかのf11点がある。それは乳
化の過程で水の添当[目1F、攪拌11.1間の設定、
反転を行わせる水量の設定なとの諸条件について、41
14めて細心の注意を要し、使用する原料特に界面活性
剤のHl、ltに関しては影響が大きく、ロットブレな
どの品質変動や作業者の技術欠除により、再現性の乏し
いものとなりがちである′且である。まだ、界面活性剤
と油相との相溶性にも影響され、相溶性が良ずきでもあ
るいは悪ずき゛ても良好なエマルションがイk)らjl
ない等の短1点が存在する。
On the other hand, as a method for producing a stable oil-in-water emulsion (1), the agent-in-oil method described above has been reported to be superior to date. This agent-in-oil method is a method in which a nonionic surfactant is dissolved in an oil phase, and then an aqueous phase is added to this oil phase to obtain an oil-in-water emulsion through phase inversion. In the production of oil-in-water type, including the above-mentioned gel emul/yono problem,
Even with this method, there are some f11 points. It is the addition of water during the emulsification process [1F, stirring 11.1 setting,
Regarding the conditions for setting the amount of water for inversion, 41
14) Careful attention is required, and the raw materials used, especially the surfactants Hl and Lt, have a large influence, and reproducibility tends to be poor due to quality fluctuations such as lot fluctuations and lack of skill on the part of the operator. ′And it is. However, it is still affected by the compatibility between the surfactant and the oil phase, and whether the compatibility is good or bad, a good emulsion can be obtained.
There is one short point such as "no".

本発明者等は、上記諸点を解決するため鋭意研究した結
果、界1M1活性剤中油型ゲル状エマル/ヨノを利用す
ることによ1ノ、粒子が均一で極めて細かく、過酷条件
下でも安定なゲル状エマルソヨンと水中油型エマルシヨ
ンが得られると共に、従来になく再現性の良い簡易な製
造法を完1J又しだのである。
As a result of intensive research to solve the above-mentioned problems, the present inventors have found that by using KAI 1M1 activator oil-in-gel emul/Yono, the particles are uniform, extremely fine, and stable even under harsh conditions. A gel-like emulsion and an oil-in-water emulsion can be obtained, and a simple manufacturing method with better reproducibility than ever before has been completed.

本発明はグリコール4j寸だに[ぞ0詩導体の1イlT
i捷だd、その1.f55部の1打あるい(・:j、2
紳以1から選択された水溶性R’r媒と水から7′I:
ろ水相成分と非イオン界面活性剤とを溶)竹して界面話
+1削連続相を作製し、次いで油相成分6−・添加I−
トシめて界面活性耐相中油よりに:るケ九仄−I−,’
 ノ1 ’7 :1ンをイ(Iることを特徴とするゲル
状r−、−jl ’7・1)の製造法に関する。
The present invention is glycol 4j size [zo0 poem conductor 1ilt
i kadad, part 1. f55 part 1 stroke or (・:j, 2
From a water-soluble R'r medium selected from XI and water 7'I:
Dissolve the filtered water phase components and the nonionic surfactant) and prepare a continuous phase by removing the interfacial layer +1, and then add the oil phase components 6- and 1-.
From surface-active phase-resistant medium oil:
The present invention relates to a method for producing gel-like r-, -jl'7.1, which is characterized in that ノ1'7:1.

さらには、に記、’i(1! ?ii、法でイ!# 1
.’、)11ノ、−ケル(入−1フルンヨノに水相を添
加して連続相を界面/、I’i l’l削相から水に変
化させて水中油型−「−2ル/・1)を1することを特
徴とする水中油it、’!、 :r−lル/′−1ノの
製造法に関するものである。
Furthermore, 'i(1!?ii, law!# 1)
.. ', ) 11, -Kel (In-1 Add aqueous phase to Furunyono to change the continuous phase from the interface/, I'i l'l removed phase to water to create oil-in-water type - '-2 L/. The present invention relates to a method for producing oil-in-water it,'!, :r-l/'-1, characterized in that 1) is reduced to 1.

本発明に係るゲル状ニーJルン三17の製、;/lL法
を詳細に述べると、水溶性溶媒と水が;う 7部から8
!2部の範囲からなる水相成分にJ1イ到ン界面活性剤
を溶解させだ界It’ll /V性削相に油相を攪拌し
ながらゆっくり添加していき、界自活性剤相中油よりな
るゲルエマル/ヨ/をf′1成する工(11″か【)な
る3、木下4:’【!におい、てQ−1、油相をゆっく
り添加し、でいき、1分に界面詰性剤連h゛シ相に油相
6−分1枚させる1、こJlに、1.す、界面活イ′1
−削と浦の71!−面張力が1鋒に小さく、1.11s
 Fl、じ相が水の、1ノ、)音、I−比べずつと細か
い乳fし詔jがイ’j、 (7,、I する/、−め、
乍1別のホ1−ゲーノーイ11゛−伏11の機(11(
シ眉I′/1′6−1・11わ4: < −Cイ1.4
@j 、V’)て細かい1勺″1′↓:+−,・ル、・
・Iン介′谷易C〈−イ:Iることがてきる1、こ7t
 hのIN“l’、 i<+、・ける水/1存41溶媒
。1−水の割合tit前記のill’lす、37部か”
) 8 ’、 2部であるIV・安かあ;二〕、水が7
割で1) +Iイイえ/)占ツメノー1.・、Lひ−\
ギリゴー・(液晶が出現する1、水τ′17割を、[イ
イえしかも界曲話+l剤のl11.l+飴が7〜1′2
31比1に的低い、甲1合i1/iメラー鍼品相11゜
なる4、ンメ′ノー戯晶Q−し!・:1;の油を溶館N
 L、でし1い、油相庖添加するだけで&:t W面l
l’l性剤中油)(/JJlji7′:IVと01、な
らない、界面話+1゛削のl l l−、i・値が12
より高いJll+j合&J1、−\ギーリゴーノ1液晶
の−jl常にイ便いゲルが出現し、そこに油相を分散さ
せることがJl常に%Ill L、い1、−力、水溶性
溶媒に対し水の割合が2未/1νりの」4.ら合(・−
」1、界面活t」削が水−水溶f1溶媒中で会合゛J−
ること乙・く分J′漕its’(1−t−いるものと思
わjl、ミセル形成も灯わIl、 :4’、い1.1:
σ)/、−め、油相・\のl/′ド而縞面削の吸4′’
、: 、1/lか低l−1、うル状(1) W 1rl
l 話(’l削相中油:+: −、) /L /1−6
川?成−11−J゛、(1(1′lllの油分11り糸
かf!) l’+ :11/:、u)ツノ−“C−11
・・・、1かかる二IJ、 、;、l、jに1.・け/
[)水相に7容j蝉−、ト/、)]厚]川用1’i (
’l I’?’l r、12()申:1:%]゛ツ、1
.−’C8Fl中111係以1・−C7(・)/:、ノ
1<・′叔が5ら/′)、、′!()中・1:%以1・
Cあ;:)、L: W−lii話1’l削(目111層
jl“t)(ll?;形成1− /C,ことかできJ−
1水溶(’l溶II、1(、(−曲(11が分子!’f
 l−7+−状pj1:(1,二、へってし7−11い
、ウノ【仄−1°・ノ【/!7・tl、片3成バ\i+
/′:い3.ノl′/!に80中’1’: z以Iでイ
、h′[″面乱□−II削i1.S セ/L、会合?、
1l11..I’ コ、lカー(、% ;4. イ;:
 思わJl、ケル状上マル/−I〕11、形成t〜)1
ろ“い、。
To describe in detail the method for producing the gel-like knee gel according to the present invention; 7 to 8 parts;
! Dissolve the J1 polymer surfactant in the aqueous phase component consisting of 2 parts and slowly add the oil phase to the surfactant phase while stirring, and remove the surfactant from the oil in the surfactant phase. Gel emul/yo/ is formed f'1 (11'' or [) Naru 3, Kinoshita 4:' [! Odor, Q-1, oil phase is slowly added, and the interfacial packing property is increased in 1 minute. 1. Add 1 layer of oil phase to the drug continuous phase.
-Share and Ura's 71! - Surface tension is as small as 1.11s
Fl, the same phase is water, 1 no, ) sound, I- Comparatively finer milk f is I'j, (7,, I do/, -me,
11 different ho 1 - game noi 11 ゛ - down 11 machine (11 (
ShibyouI'/1'6-1・11wa4: <-Ci1.4
@j , V') and detailed 1"1'↓: +-,・le,・
・Insuke'Taniyoshi C〈-I: I can come 1, this 7t
h IN "l', i<+, ・Water/1 remaining 41 solvent. 1-Ratio of water tit the above ill'l, 37 parts"
) 8', 2nd part IV Yasukaa; 2], water is 7
1) +I good/) fortune telling 1.・、Lhi-\
Girigo (liquid crystal appears 1, water τ' 170%, [good and Kaikyu story + l agent l11.l + candy 7~1'2
31 ratio 1 is low, A1 go I1/I Meller acupuncture phase 11° 4, Nmen'no play crystal Q-shi!・:1;
L, 1, just add oil phase &:t W side l
l'l l' l l l l-, l l l-, i value is 12.
The higher the Jll + j + J1, -\ Girigono 1, the -jl of the liquid crystal always appears, and the dispersion of the oil phase therein is Jl always % Ill L, I1, - force, the water relative to the water-soluble solvent. 4. The ratio is 2/1ν. ra (・-
"1. Surface active t" decreases association in water-aqueous f1 solvent ゛J-
It seems that there is a possibility of micelle formation. : 4', 1.1:
σ) /, -me, oil phase / \'s suction 4''
, : , 1/l or low l-1, fibrous (1) W 1rl
l story ('l removal phase oil: +: -,) /L /1-6
river? Sei-11-J゛, (1 (1'lll oil content 11 thread or f!) l'+ :11/:, u) Horn-"C-11
..., 1 takes 2 IJ, , ;, 1 for l, j. ·hair/
[) 7 volumes in the aqueous phase, t/,)] thickness] 1'i for rivers (
'I'? 'l r, 12()mon:1:%]゛tsu,1
.. -'C8Fl中111 1・-C7(・)/:、ノ1<・'下が5ら/′)、、′! () Medium・1: % or more 1・
Ca;:), L: W-lii story 1'l cut (eye 111 layer jl "t) (ll?; Formation 1- /C, Kotokade J-
1 water solution ('l solution II, 1 (, - song (11 is the molecule!'f
l-7+-like pj1: (1, 2, heteshish7-11i, Uno [组-1°・ノ[/!7・tl, piece 3 formation bar\i+
/': 3. Nol'/! '1' in 80: z to I, h'[''menran□-II cut i1.S C/L, meeting?
1l11. .. I' ko, l car(, %; 4. I;:
I think Jl, Kel-like upper circle/-I] 11, formation t~) 1
Ro“i,.

本発明ゲル状エマル7丁1ノの1′1成C(1,・い−
(用いら71ろ水相成分とじての水溶1′1溶媒v、1
、l11にグリコール入臼−オ/1−シj、ぞの1、ん
導1本かンy・げ”+71、例えば、ブ[lビレ/グリ
:ノー11.11,3−)IIバッジオール、l、;3
−ブタ/ジオール、1,1 −ツクノンオール、1.5
−ペンクン/オール、+−f−レ/クリコールへY?の
ダリ=1−ル類、ゾ;■−チレ/クリ−I−/l/、l
−リx−f−レンクリコール、ホリエチレノグリコール
(平均分子情300以下)、ジグロビレノグリコールな
どのグリコール誘導体等であり、これらを一種または二
種以上を選択して用いるものである。か\る必須成分と
しての水溶性溶媒に加え、ゲル状エマルンヨンを崩壊し
ない程度てあれば、必要に応じ、化粧品、食品等の各種
製品に配合される他のどのような水溶性溶媒も併せて利
用することができる。
7 gel emuls of the present invention 1'1 composition C (1,・I-
(Used 71 filtrate phase components as water soluble 1'1 solvent v, 1
, l11 glycol injected / 1-shij, 1, guide 1 kany・ge"+71, for example, bu [l bire/gri: no 11.11, 3-) II badge all ,l, ;3
-buta/diol, 1,1-tukunonol, 1.5
-Penkun/all, +-f-re/Krikor to Y? Dari = 1-l, zo;■-Chile/Cli-I-/l/,l
These include glycol derivatives such as -lyx-f-lene glycol, polyethylene glycol (average molecular weight: 300 or less), and diglobyreno glycol, and one or more of these can be selected and used. In addition to the water-soluble solvent as an essential ingredient, any other water-soluble solvent that is blended into various products such as cosmetics and food may be added as necessary, as long as it does not disintegrate the gel emulsion. can be used.

本発明に適用される非イオン界面活性剤d1、tl 1
訂値を5.5から18に調整したものが一種捷たは2秒
以上を混合して用いられる。H1訂(値が5.5未a〜
のものは油相が界面活性耐相に溶解してしまうだめ、ゲ
ル状エマル7ヨンが得られない。逆に、18を超える場
合油相への吸着性が低下するため、これもゲル状エマル
ションとはならない。具体的な非イオン界面活性剤とし
ては、ソルビタン脂肪酸エステル、ポリオキンエチレン
ソルビタン脂肪酸エステル、グリセリン脂肪酸エステル
、ポリグリセリン脂肪酸エステル、グリセリン脂肪酸エ
ステルの酸化エチレン1.4導体、プロピレングリコー
ル脂肪酸ニスデルの酸化エチレン誘導体、プロピレング
リコール脂肪酸ニスデル、ポリエチレ/ダリニ!−ル脂
肪酸エステル、ポリエチレノアルキルエーテル、ポリオ
キンエチレンアルキルエーデノシ、ホ1)−)、−゛/
グロビレンアルキルエーテル、ホ’) オ’r /ニー
1−レンアルキルフェニルエーデル、ポリ」ギ/nチレ
ンヒマ/油誘導体、ポリオキ/エヂレノ硬化ヒマ/油誘
導体、ポリオキ/ニー1゛レノノイトスタノール、フィ
トステロール゛r1が)7−は1ン11、これらを−オ
車捷たは一4中で目的のものが(!) B:)ねない場
合には二種以ト組合すて用いるもヴノであり、本発明に
おける使用h4°d、従来の乳化法とくらベア0係程度
以「でよい。(従って、界面話(1剤の使用による皮膚
刺激、皮11−71・・1・害す1−・〕“J fl(
71,l<肴−図ることができ、安全性に優れA−もの
rtイ”するl二とが可能である。) 寸た油相成分に用いる油剤としてCF、 Jlji ′
7;’Iのイ。
Nonionic surfactants d1, tl 1 applied to the present invention
The one with the correction value adjusted from 5.5 to 18 is used in combination with one type or more than 2 seconds. H1 edition (value is 5.5 or less)
In this case, the oil phase dissolves in the surfactant phase, and a gel-like emulsion cannot be obtained. On the other hand, if it exceeds 18, the adsorption to the oil phase decreases, and this also does not result in a gel-like emulsion. Specific nonionic surfactants include sorbitan fatty acid ester, polyquine ethylene sorbitan fatty acid ester, glycerin fatty acid ester, polyglycerin fatty acid ester, ethylene oxide 1.4 conductor of glycerin fatty acid ester, and ethylene oxide derivative of propylene glycol fatty acid Nisder. , propylene glycol fatty acid Nisder, polyethylene/dalini! -3 fatty acid ester, polyethylene alkyl ether, polyethylene alkyl ester, ho1)-), -゛/
Globylene alkyl ether, H') O'r/N-1-lene alkyl phenyl ether, Poly-G/n-Tyrene castor/Oil derivative, Polyoxy/Edilene hydrogenated castor/Oil derivative, Polyoxy/N-1-Lenoinoitostanol, Phytosterol r1) 7- is 1-11, and if you can't get the desired thing (!) B:) by changing these - or 14, it's no good to use two or more of them together. , the use in the present invention h4°d, compared to the conventional emulsification method, may be less than 0. ] “J fl(
CF, Jlji' as an oil agent used for small oil phase components.
7;'I of I.

のでよく、スクワラン、流動パラフィン、ワセリノ、オ
リーブ油、グリセロールトリス−2−エチルヘキザノエ
〜1・、ミックオイル、イノゾロビルミリステート、ミ
リスチン酸ミリスチル、オレイノ酸オクチルトテヵノー
ル、ホポハ?由、ミノロウ、ラノリン、メチルポリンロ
キザン等が挙げられ、特に好ましくは炭化水素系とエス
テル系油剤であり、トリグリセライドの使用にあたって
d:これらと併用するものである。
So, squalane, liquid paraffin, Vaseline, olive oil, glycerol tris-2-ethylhexanoe~1, Mic oil, inozolovir myristate, myristyl myristate, octyl totecanol oleinoate, hopoha? Among them, hydrocarbon-based and ester-based oils are particularly preferred, and these are used in combination with triglyceride.

次に、本発明の第一段階(ゲル状エマル/ヨンの作成)
における水の使用が有効なJj1由について、水を用い
る場合と用いない場合の溶解性の違いを相平衡図を用い
て個へた結MJ:をi〈l −]校び図−2に示す。界
面活性剤としてポリオキンエチレン((し)オレイルエ
ーテル、油剤ハ流動ハラ7 イン、水溶性g6F:j:
 ]、:(−グ′7ンソオール、−用いた。図−1i水
相として1,3−フリツノオールを用いた系の相図であ
る。1,3−ブタ7ノオールとポリオキンエチレ7 (
G+オレイルエーテルは溶解しあい、無色透明溶液を示
す。こ\に流動パラフィンを添加していくと、初めは溶
解して行くが、飽和性γjj(度以十に乙−ると分肉1
(シて、流動パラフィンと1,3−ブタン7月−九・岑
面活1生剤m液に分かれる。この分流・唄域にし1′汐
、定なケル状エマルンヨノは存在しない4、−ツバ水)
111として水と1,3−ブタノンオールを1iliT
l−ii−i−比で用いた場合は、]、;]3−フク/
ソーシール水・界+rn活性活性剤溶流動バシフィ/苓
、添加すると初め(寸図−1と同様に無色透明 相を・
1ずが、さらに流動パラフィンが冷加さ才L−(−分V
:lt ’iiJ″J域になると、この領域の−7<1
i (、・Lニケルエ−Jノトンヨ1]をンドず部分が
現われる6、ケル状−「マル/;1ノは無色透明あるい
は青白色透明で、)1 ′7:;に粘度が高い状態を示
している。こXに水相を加えることによって微細な水中
油型エマル/コンが(’V ’、+れる。ゲル状エマル
/ヨンを/J−さないf+f′jh:Q k・−水相を
添加しても微細]な水中油Lζ1jエマ几/ヨ7ノ(r
l:イlIられない。水相として水溜性溶媒のみろ用い
た場合と水溶性溶媒と水をf、If川しY−場合のJJ
uψの違いは、非イオン界面活性剤の会合(/(=、L
iオる影響の差に起因しているものと考えられる71才
なわち、水を併用することにより、界面活性剤の会合を
適当に促し、油表面への界面活性剤の吸着をより向トさ
せ、細かい油滴を七1つだゲル状エマル/ヨンを力える
ことになる。それと同時に界m1活性剤相を低濃度域寸
で広げている。
Next, the first step of the present invention (creation of gel emul/yon)
Regarding the reason why the use of water is effective in Jj1, the difference in solubility between when using water and when not using it is shown in Figure 2 by using a phase equilibrium diagram to calculate the individual hetadion MJ: i〈l −]. . As a surfactant, polyethylene ethylene ((shi)oleyl ether), oil agent (fluid Hala 7in), water-soluble g6F:j:
], :(-g'7-ol, - was used. Figure 1i is a phase diagram of a system using 1,3-fritnool as the aqueous phase.
G+ oleyl ether dissolves into each other, giving a colorless and transparent solution. When liquid paraffin is added to this, it will initially dissolve, but the saturation
(The liquid paraffin and 1,3-butane are separated into liquid paraffin and liquid paraffin.There is no definite gel-like emulsion in this branch/singing area.) water)
1iliT of water and 1,3-butanoneol as 111
When used in l-ii-i- ratio, ],;]3-fuku/
When Saw Seal Water Kai + RN Activator Solution Liquid Bacify/Rei is added, it initially forms a colorless and transparent phase (same as Dimension 1).
1. Then, the liquid paraffin is further cooled.
:lt 'iiJ''When it comes to J area, -7<1 in this area
i (,・Lnickel-Jnotonyo1] 6, kel-like - "maru/;1" is colorless and transparent or bluish-white and transparent,)1 '7: ; indicates a state of high viscosity. By adding an aqueous phase to this, a fine oil-in-water emul/con is produced ('V',+). Oil in water Lζ1j Emma 几/YO7ノ(r
l: I can't do it. JJ when only a water-retaining solvent is used as the aqueous phase and when a water-soluble solvent and water are used as f, If river and Y-
The difference in uψ is due to the association of nonionic surfactants (/(=, L
This is thought to be due to the difference in the effects of water on the surface of the oil. This will force the gel-like emulsion to form fine oil droplets. At the same time, the surfactant m1 active agent phase is expanded in the low concentration range.

水溶性溶媒たけでは、非イオン界面活性剤がミセルを形
成しにくいことはhイに文献にも報告されている。(+
’(、Rigamont+ 、M、 T、 Ceret
i Mazr、a、。
It has been reported in the literature that nonionic surfactants are difficult to form micelles in water-soluble solvents. (+
'(, Rigamont+, M, T, Ceret
i Mazr, a.

Hiv、 Ttal、 5oStanze 0rass
e+ 4L 532 (1970))。
Hiv, Ttal, 5oStanze 0rass
e+ 4L 532 (1970)).

J)J上示ずように、水溶性溶媒と水を混合させて界面
活性剤の油滴への吸着性を高め、微細なゲル状エマルン
ヨノを形成させている。(逆に水だけだと界面活性剤は
無限に会合してし甘い、液晶を形成してしまう。液晶は
非常に硬度が高かったり、゛合一安定性が悪いため油相
を敵晶中に均一に分散させることが困難な場合が多い。
J) J As shown above, a water-soluble solvent and water are mixed to increase adsorption of the surfactant to oil droplets and form a fine gel-like emulsion. (On the other hand, if there is only water, the surfactant will combine indefinitely and form a sweet liquid crystal.Liquid crystals have very high hardness and poor coalescence stability, so the oil phase is mixed into enemy crystals.) Uniform dispersion is often difficult.

)かくして、本発明に係るゲル状エマルンヨンは合一に
対して安定であるため、製造工程における諸条件、例え
ば攪拌速度、時間、温度、装置等の制約を受けることが
少なく、より容易に安定な0ハVエマルンヨンの製造か
【1]能であると同時にゲル状エマル/ヨ/そJ1自体
を製品としてル」川することができる1、 まだ、かXるケル状エマル/ヨ/IL、これに水相を添
加して製造される水中油型」−マル/ヨンを得るために
心火であるはがりて、(<、さらに優れた特徴を有する
ものである。、これi −Cili販されているゲル状
のクレン・/ンククリーノ3、コールトクリーノ・等は
油分や界面活1′1剤の配合稙が多量に用いられている
ため、皮面VC塗イIJされた後にこれを払拭する場合
、水で洗い落すことは不可能であり、通常は水41−洗
顔料を用いることによって初めて皮肉に残存した化41
1品内存物を洗い落すことができ/)1.これに付し、
本発明の場合このような水性法に(見料を用いることろ
・く、水だけの使用により容易かっき11.いに内界物
を払拭することがてきる。
) Thus, since the gel-like emulsion according to the present invention is stable against coalescence, it is less subject to restrictions on various conditions in the manufacturing process, such as stirring speed, time, temperature, equipment, etc., and it is easier to create a stable gel. It is possible to manufacture gel-like emulsions and at the same time produce the gel-like emuls/yellows themselves as products. It is an oil-in-water type oil-in-water type produced by adding an aqueous phase to the oil-in-water type, which has even more excellent characteristics. Gel-like cleaners such as CLENE/NCCLINO 3, COOLTO CLEAN, etc. contain a large amount of oil and surfactant 1'1 agents, so this should be wiped off after applying VC to the skin. ironically, it is impossible to wash it off with water, and it is usually only by using water-41-facial cleansers that the remaining chemical-41
You can wash off the contents of one item/) 1. Along with this,
In the case of the present invention, it is possible to easily wipe away internal substances by using only water, instead of using such an aqueous method.

次は、本発明のもう一つの[[的である水中油型エマル
/コンの製造法であるが、I−配下4“ijて得られた
ゲル状エマルショ/に水せ/−(寸必−要に応じて水溶
性添加物を溶解し、た水相を加えて、連h′し相を11
1面活性剤から水へと連続的に変化さぜ、水中油型エマ
ル/ヨ/をイ:Iる方法である。
The following is a method for producing an oil-in-water emulsion/container, which is another target of the present invention. If necessary, dissolve the water-soluble additives, add the aqueous phase, and continue to heat the phase for 11 hours.
This is a method of converting a surfactant into water continuously to create an oil-in-water emul.

この云わば第−ユニ4゛1″に′1・・ける水相成分の
添加方法としては徐々に添加することか灯1しく、こi
t V?:よらない場合に&′j 、優拌に長期間と強
力な機械力などの援助を一安求され、必ずしも効−矛′
的なものと云えなくなるばかりでなく、イ1)られるエ
マル737粒子か大きくなりゃすい。水相成分としてr
ll、水単独か又d2水と他の水溶性成分の混合水溶液
が挙げられる。基体的な水溶イイ4−成分とし−Cば、
IT、 iiLi一段階のゲル状エマル/ヨシて必須成
分として用いる水溶性溶媒の他に、各神製品に用いられ
ている通常の水溶性成分でよく、例えはグリセリン、ジ
グリセリノ、ソルビト−ル、マルチト−ル、エタノール
、ムコ多糖力゛J、乳酸すトリウム、パンテチ/、ピロ
リド7カルボ/酸ナトリウノ、等が挙げられる。
In other words, the best way to add the aqueous phase component in Unit 4'1'' is to gradually add it.
t V? : In case of failure, assistance such as gentle stirring for a long period of time and strong mechanical force is required, and it is not necessarily effective.
Not only will it no longer be possible to say that it is a typical particle, but the Emul 737 particles that can be used will become larger. r as a water phase component
ll, water alone or a mixed aqueous solution of d2 water and other water-soluble components. As the basic water-soluble 4-component -C,
In addition to the water-soluble solvent used as an essential ingredient in IT, iiLi one-stage gel emul/Yoshi, ordinary water-soluble ingredients used in each product may be used, such as glycerin, diglycerino, sorbitol, and malt. -ol, ethanol, mucopolysaccharide triglyceride, sodium lactate, pantethyl, pyrrolido 7carboxylic acid, and the like.

かくして第一エイ−“tと第」一工程を経て得られる水
中油型エマル/ヨシは粒子が均一で、極めて細かく、J
F’j r’i:’ii件下においてもかなり安定式も
のが提供される6゜ 従来、ニーフル7ヨノのイ′[製にあ7/6−リ、水溶
1′1溶媒を応用した報告frl、いくつか兇t、′I
する1、1り1j;、乏し11、特開昭51 5578
.’(シじ゛に」、・いてifl、安定A゛水中油型至
マル/ヨノの製J<1□十イ′1″で水溶1′l溶々]
1)、中油エマル/ヨシを作製し、そ;7+、”f+)
水て怖釈−J゛る方法を用いている。さらに1.X11
9.:1・;l n11.+ tLi’、’i水水性溶
媒中玉エマルションついて(′1・、i /+1.1で
いる1、特開昭51−5578:3号でit水溶慴溶〃
1!1、中油1(りエマル7′−Jンを作る[−1的で
水溶性溶媒か用い”J i−+ている3、これに対し、
本発明に1゜−いて水と水溶1/1溶媒を用いる[1的
は、界面活1/1削6−・ミセル会合させ、しかも液晶
を形成させることなく界面liら付則連続相をつくるこ
とにある1、従って第 [−イー7で(4)られるゲル
状エマル/ヨシV1、界面話件削相中油型であり、水溶
性溶媒中浦型−T−マル/Elンとはそのメノノニズl
、が異なるものである3、さらに、本発明に係る製j置
去と特開昭51 5578.’3号の方法のメカニズム
が猫なる点d1、第一段階において水の使用が必須条件
であるとと\、水溶性溶媒中油シ1.リエマル/ヨノで
はないため、界[f1目1′!I性剤の会合を促すグリ
コール類及びその誘導体が特に利用可1+ヒであるとい
う点にあり、特開昭51−5578:3号の方法が水溶
イつ、溶媒中油という点から、必須成分としてメタノー
ル、エタノール、グリセリン等のあらゆる水溶性溶媒を
オIj用できる点からみても、本発明のメカニズムが異
なるとア4I解できる。このように本発明はこれ捷でに
ない新しい方法によって良好な水中油型を外− エマル/ヨシを製造する方法を提供するものである。
In this way, the oil-in-water emul/reed obtained through the first step of ``T and 1st'' has uniform particles and is extremely fine.
F'j r'i: A fairly stable formula is provided even under 'ii. frl, some, 'I
Suru 1, 1ri 1j;, Kashi 11, JP-A-1978 5578
.. '(Shijini', ifl, stable A゛Oil-in-water type extremely/Yono's production J<1□10'1'' water-soluble 1'l melted)
1) Make a medium oil emul/reed, then; 7+, "f+)
He uses a method called water test interpretation. Furthermore 1. X11
9. :1・;l n11. + tLi', 'i for the emulsion in the water aqueous solvent ('1., i /+1.1 1, JP-A-51-5578: No. 3)
1! 1, make a middle oil 1 (reemul 7'-J) [-1 using a water-soluble solvent] 3, on the other hand,
In the present invention, water and a water-soluble 1/1 solvent are used [one purpose is to reduce the surface activity by 1/1 and cause the micelles to associate, and to create a continuous phase at the interface without forming liquid crystals. 1, therefore, the gel-like emul/Yoshi V1 represented by (4) in [-E7] is an oil type in the interfacial case, and the water-soluble solvent Nakaura type-T-Mal/Eln is its menononizl.
, are different. 3. Furthermore, the manufacturing method according to the present invention and JP-A-51-5578. The mechanism of method No. 3 is a cat d1, the use of water is an essential condition in the first step, and the use of oil in a water-soluble solvent1. Because it is not Riemal/Yono, Kai [f1 eyes 1'! Glycols and their derivatives that promote the association of I-sex drugs are particularly useful, and the method of JP-A No. 51-5578:3 uses water-soluble compounds and oil in the solvent, so that glycols and their derivatives can be used as essential components. Considering that all water-soluble solvents such as methanol, ethanol, and glycerin can be used, it can be understood that the mechanism of the present invention is different. Thus, the present invention provides a method for producing a good oil-in-water type emul/reed by a unique new method.

仄に本発明に係る水中油型エマル7ヨノが如何に微細な
ものであるかを実証するだめ、捷ず本発明界面活性剤相
中油エマルンヨ/の状態を示した電子顕徴税写真(倍4
< : ] (1、000倍)を図=3(略)に示す。
In order to subtly demonstrate how fine the oil-in-water emulsion according to the present invention is, an electron micrograph (magnification 4
< : ] (1,000 times) is shown in Figure 3 (omitted).

組成は非イオン界面活性剤としてポリオキンエチレノオ
レイルエーテルを用い、油相成分として流観1パラフィ
ン、水溶性溶媒として1.:3−ブタンジオールを用い
タモ(7)である。写真に示すように油のわ“’71’
 &−:を約0.2μIll程度で極めて細かい乳化r
1%I ’5 yJ、している6、−また乳化制はクロ
ーズドバックの状態に品って1.・す、これがゲル状を
形成している理由とf、〉’H−L:、れる。
The composition uses polyoxine ethylene oleyl ether as a nonionic surfactant, 1 paraffin as an oil phase component, and 1. : Tamo (7) using 3-butanediol. As shown in the photo, Yunowa “'71”
&-: extremely fine emulsification of about 0.2μIll
1% I'5 yJ, 6, - Also, the emulsification system is in a closed back state.・Why does this form a gel?

さらに、この界面活付削相中油ニーlル/口/に水を添
加して水中油型エマル/=+7J: L /i−、J混
合のIIr+微鏡写真を図−・1(略)に及O・111
1′畠の1’−−・/エツトインオイル法を用いて乳化
し、さらにホモミキザーで10,00081’す・、4
.5分間乳化し/、−エマル/ヨシの顕微鏡′Lj直を
図−5(略)に/j、ず。図−・1と図−5のb′真を
比軸−1−ると、校了の大きさや均質性において本発明
の力θユか数段すぐれたものであることに1、明白であ
る、。
Furthermore, water was added to the oil in the surface-activated cutting phase to form an oil-in-water emulsion /=+7J:L/i-, a microscopic photograph of IIr+ of the J mixture is shown in Figure 1 (omitted). O・111
1' Emulsify using Hatake's 1'--/Et-in-oil method, and further add 10,00081' with a homomixer.
.. Emulsify for 5 minutes and observe the emulsion under a microscope in Figure 5 (omitted). If we compare b' true in Figures 1 and 5 with the ratio axis -1, it is clear that the power of the present invention is several orders of magnitude superior in terms of the size and homogeneity of the proofreading. ,.

本発明のゲル状エマル/ヨノ分−形成させる場合には、
前述した如く水相成分11C、t・ける水溶(1溶媒、
水、非イオン界面活性剤・))各成分イし調整すべきで
ある。このような構成72分の比、(′C1水溶性溶媒
:30〜80部、水20〜70部、界面話4′1斉11
 :J〜80部で、好寸しくは各々210〜70部、;
う()〜()0部、30〜60部である。この範囲は油
相を添加してゲル状エマルションを得るだめの至適量で
あり、これによらない場合ゲル状エマルンヨンを生成し
にぐいものである。第一工程において添加される油相量
は、上記界面活性剤連続相に対して130〜95重量%
で、好ましくは70〜00重量係である。この範囲もや
はりゲル状エマルンヨンを与える範囲である。しかし、
界面活性剤の目的からすれば如何に少量で多量、の油相
が乳化できるかが大切であるから、良好な水中油エマル
ションをイIIるにはに限の範囲が重要となる。(多量
の界面活性剤を使うならば、水沫によらなくても容易に
水中油型エマルションをイ4)ることができるからであ
る。) 第二工程において水相成分を添加する際に留意すべきこ
とは、既に前述した如く、徐々に水相をゲル状エマルシ
ョ/に添加することが好寸しい。徐々に水相成分を添加
させることにより、ゲルがままこ状に水相に分散するの
を防ぐと共に、乳化滴の成長を抑制するためでもある。
In the case of forming the gel-like emul/yono component of the present invention,
As mentioned above, the aqueous phase components 11C, t.
Water, nonionic surfactant, etc. Each component should be adjusted accordingly. Such a composition ratio of 72 minutes, ('C1 water-soluble solvent: 30 to 80 parts, water 20 to 70 parts, interface talk 4'1 ratio 11
:J~80 parts, preferably 210~70 parts each;
U() to ()0 parts, 30 to 60 parts. This range is the optimum amount for obtaining a gel-like emulsion by adding the oil phase; otherwise, it is difficult to form a gel-like emulsion. The amount of oil phase added in the first step is 130 to 95% by weight based on the surfactant continuous phase.
The weight ratio is preferably 70 to 00. This range also provides a gel-like emulsion. but,
From the viewpoint of the purpose of the surfactant, it is important to be able to emulsify the oil phase in a small amount and in a large amount, so a limited range is important in order to obtain a good oil-in-water emulsion. (If a large amount of surfactant is used, an oil-in-water emulsion can be easily formed without using water droplets). ) When adding the aqueous phase components in the second step, it should be noted that, as already mentioned above, it is preferable to gradually add the aqueous phase to the gel emulsion. By gradually adding the aqueous phase components, it is possible to prevent the gel from being dispersed in the aqueous phase in a lumpy manner, and also to suppress the growth of emulsified droplets.

また水相成分の添加量に対しては範囲を設ける必要はな
いが、水中油型エマルションをイ!Iるのに許容される
至適量が用いられる。
Also, there is no need to set a range for the amount of water phase components added, but oil-in-water emulsions are recommended! The optimum amount tolerated by the patient is used.

上記の如くしてイ;Iられる水中油型エマル7ヨンは乳
化粒子が殆んど095μI11以1・の細かい極めて均
一なものであり、エマルンヨ/の安定1シ1は通′、;
δの方法によりイIIられだエマルノコ/と比較しては
るかに安定であり、特に高?int (1111Kふ・
ける安定性は従来になく優れたものである。
The oil-in-water emulsion prepared as described above has very fine emulsified particles of almost 0.95 μl or more, and is generally stable;
Due to the method of δ, it is much more stable compared to IIII Rareda Emarunoko/, especially at high temperatures. int (1111Kfu・
Its stability is unprecedented.

才だ、本発明の水中油型エマルションの製造法は各原料
の使用−量及び攪拌HJ間の細心で厳しい条件設定、強
力な機械的攪拌力などを及することのない簡易な方法で
あり、使用する原料のロットブレや作業者の技術欠除に
基<4+1現件の問題は全くなく、工業スケールでの円
、litな製造をなしイIIるものである。
The method for producing an oil-in-water emulsion of the present invention is a simple method that does not require careful and strict setting of the amount of each raw material used and the stirring HJ, and does not require strong mechanical stirring power. There are no current problems of <4+1 due to lot variations in the raw materials used or lack of technical skill among the workers, and it is possible to perform lit production on an industrial scale.

本発明に係る水中油型エマルションは、その有する利点
のため、化粧料、食111“ハゲ薬品、塗料その他各種
の用途に用いるこ々ができる。。
Owing to its advantages, the oil-in-water emulsion according to the present invention can be used in cosmetics, food products, baldness medicines, paints, and various other applications.

次に本発明ゲル状エマル7ヨノと水中油型エマルション
の製造法の実施例をンJりず3、含有割合は7Ir量係
である。
Next, an example of the method for producing a gel-like emulsion of the present invention and an oil-in-water emulsion will be described.The content ratio is based on the amount of 7Ir.

実施例1 1.3−ブタンジオール4チとn製水3チからなる水相
成分とソにビタンモノステアレート1.0%、ポリオギ
ンエチレン(20)ソルビタンモノスアレ−1−71,
O%とを100Cで加温溶解させて界面活性剤連続相を
作製する。別にスクヮラン30 % 、グリセロールト
リス−2−エチルヘキサノエート20%に適量の防腐剤
を添加した油相成分を70°Cに加温し、これを前記の
界面活性剤連続相に徐々に添加して界面活性剤連続相ゲ
ル状エマルションをイ!にる。
Example 1 A water phase component consisting of 4 parts of 1.3-butanediol and 3 parts of n-made water, 1.0% of bitan monostearate, polyogine ethylene (20), sorbitan monostearate-1-71,
A continuous surfactant phase is prepared by heating and dissolving 0% at 100C. Separately, an oil phase component prepared by adding an appropriate amount of preservative to 30% squalane and 20% glycerol tris-2-ethylhexanoate was heated to 70°C, and this was gradually added to the surfactant continuous phase. Create a surfactant continuous phase gel emulsion! Niru.

実施例2 J、3−ブタンジオール2係、ポリエチレングリコール
(200) 2%と精製水2%からなる水相成分にポリ
オキシエチレン(15)オレイルエーテル4係を70℃
にて加温溶解させて界面活性剤連続相を作成す冠。別に
スクヮグン60%、オリーブ油5チ、密ロウ5係に適量
の防腐剤、抗酸化剤を添加した油相成分を70℃に加温
溶解し、これを前記の界面活性剤連続相に徐々に添加し
て界面活性剤用中油ゲル状エマル/ヨノ6−イUる、。
Example 2 Polyoxyethylene (15) oleyl ether 4 was added to an aqueous phase component consisting of J, 3-butanediol 2, 2% polyethylene glycol (200), and 2% purified water at 70°C.
A crown that is heated and dissolved to create a surfactant continuous phase. Separately, an oil phase component consisting of 60% Squagun, 5 parts olive oil, 5 parts beeswax, and appropriate amounts of preservatives and antioxidants was dissolved by heating at 70°C, and this was gradually added to the surfactant continuous phase. Medium oil gel emul for surfactant/Yono 6-i Uru.

さらに、このゲル状エマル/ヨ/に7(1”C:の精製
水20係を徐々に添加して行き水中油型エマルンヨ/を
イ4Iる。
Furthermore, 20 parts of purified water of 7 (1"C) was gradually added to this gel-like emul to form an oil-in-water emulsion.

実施例3 L3−ブタンジオールと精製水6%からなる水相成分と
し、これにポリオ:キノエチレン(6rl)硬化ヒマ/
油4係どグリセリンスデアリフ酸ニスデル1係を80℃
にて加渦溶角(rさナーC界面活性剤連続相を作製する
。別にスクワラン:つ0%、バチルアルコール2係に適
111°の防腐剤を添加しだ油相成分を80℃に加温溶
解し、これを前記界面活性剤連続相に徐々Vこ添加して
界面活性剤用中油ゲル状エマルショ/をイIIる。さら
に、このゲル状エマルノヨンに70℃の精製水50係と
グリセリン4チの混合水溶液を添加し、て水中油型エマ
ルシ白ンを得る。
Example 3 A water phase component consisting of L3-butanediol and 6% purified water was added with polio:quinoethylene (6rl) hardened castor/
4 parts oil, 1 part glycerin dearylphate, 80℃
Prepare a surfactant continuous phase with vortex melt angle (r). Separately, add a preservative of 111° to 0% squalane and 2 parts batyl alcohol, and heat the oil phase components to 80°C. Dissolve it warmly and gradually add it to the surfactant continuous phase to prepare a medium oil gel emulsion for the surfactant.Furthermore, add 50 parts of purified water at 70°C and 4 parts of glycerin to this gel emulsion. A mixed aqueous solution of H is added to obtain an oil-in-water emulsion.

実施例4 プロピレンクリコール2%、ポリエチレ/しツクリコー
ル(200) 2 %と精製水2係からなる水相成分に
ポリオキ/エチレン(15)オレイルニーデル4%を7
0 ’Cにて加温溶解させて界面活性剤連続相を作製す
る。別にスクワランfiO%、オリーブ油5%、密ロウ
5%に適hトの防腐剤、抗酸化剤を添加した油相成分を
70 ’Cに加n1N溶解し、これを前記の界面活性剤
連続相に徐々に添加して界面活性剤用中油ゲル状エマル
/ヨンをVj)る。
Example 4 4% polyoxyethylene (15) oleyl needle was added to a water phase component consisting of 2% propylene glycol, 2% polyethylene glycol (200), and 2 parts purified water.
A surfactant continuous phase is prepared by heating and dissolving at 0'C. Separately, an oil phase component consisting of squalane fiO%, olive oil 5%, and beeswax 5% to which suitable preservatives and antioxidants were added was dissolved at 70'C for 1N, and this was added to the above-mentioned surfactant continuous phase. Gradually add the medium oil gel emulsion for surfactant.

実hiri例5 プjffピレングリコール2係と1.:3−ブタンジオ
ール2係と精製水3%からなる水相成分とソルビタンモ
ノステアレート1条、ポリオキ/エチレン(2(1)ノ
ルビタンモノステアレート4%とを70 ”Cにて加温
溶解させて界面活性剤連続相を作製する。別にスフワラ
7 :30 %、グリセロール1− IJスス−−エチ
ルヘキザノエー) 20%に適量の防腐剤を添加しだ油
相成分を70℃に加温し、これを界面活性剤連続相に徐
々に添加して界面活性剤中油ゲル状エマル/ヨンをイ;
Iる。さらに、このゲル状エマルショ/に70 ’Cの
精製水:33%と7ノルビ1〜−ル5係よりなる水溶液
4添JJt+ Lで水中油型エマルションに’ (!)
 ル。。
Actual example 5 Pyrene glycol 2 and 1. :Aqueous phase components consisting of 2 parts of 3-butanediol and 3% of purified water, 1 part of sorbitan monostearate, and 4% of polyoxygen/ethylene (2(1) norbitan monostearate) were dissolved by heating at 70"C. Separately, add an appropriate amount of preservative to 30% Sufuwara 7, 20% glycerol 1-IJ susu-ethylhexanoate, and heat the oil phase components to 70°C. This is gradually added to the surfactant continuous phase to form an oil-in-surfactant gel emulsion.
I. Furthermore, this gel-like emulsion was made into an oil-in-water emulsion by adding 4 JJt+ L of an aqueous solution consisting of 33% purified water at 70'C and 5 parts of 7 norbiol (!)
Le. .

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

図−1はポリオギ/エチレ7 ((il @レイルニー
デル・]、:]3−ブク/ジオール流動・・ラフイン系
の・10℃おける相平衡図、図−2シ1、ポリオキ/エ
チレン(6)オレイルエーテル・17.3−ブク/ジぢ
−ル・水・流動パラフィン系の小1”にに1、・ける相
平衡図とゲル状エマル/ヨ/の領域を示(〜/にもので
ある。 手   続    補   正    書  (方 式
)昭和57年72月2’7日 特許庁長官  若 4′:二 和 夫  殿■事件の表
示 昭和37年特許願第1に93g7号 2、発明の名称 ケル状エマル/ヨ/及び水中油型エマルションの製造法
3補正をする者 事件との関係    特許出願人 住所  静岡県静岡市弥生町六匹へ番地名称 ポーラ化
成工業株式会社 (同日付特許出願人名義変更届提出) 4代 理 人 住所  東京都千代田区麹町3丁目λ番地相〃第一ビル 電 話 (,26S)9乙11.9 5、補正命令の日付 昭和S7年//月/、2日 (発送日:昭和37年/7月30日) 6、補正の対象   願書、明糾1 ”t+全之及び図
面7、補正の内容 願μ+、明細書及び図面の浄iIF (内容に麦史なし
)以   上
Figure 1 shows the phase equilibrium diagram at 10°C for the polyoxy/ethylene 7 ((il @leilneydel), :] 3-book/diol fluidity... rough-in system, and Figure 2 1, polyoxy/ethylene (6) oleyl. The phase equilibrium diagram of the ether/17.3-book/diyl/water/liquid paraffin system and the region of gel-like emul/yo/ are shown. Procedural Amendment (Form) December 2, 7, 1980 Director General of the Patent Office Waka 4': Mr. Kazuo Ni ■Indication of the Case 1962 Patent Application No. 93g7 No. 2, Name of the Invention Relationship with Emul/Yo/ and the Case of Person Who Amends Manufacturing Method for Oil-in-Water Emulsion 3 Patent Applicant Address Rokutohe, Yayoi-cho, Shizuoka City, Shizuoka Prefecture Street Name Pola Chemical Industries, Ltd. (Same Date Patent Applicant Name Change Notification (Submitted) 4th Director Address: 3-chome, Kojimachi, Chiyoda-ku, Tokyo Address: First Building Telephone: (26S) 9 Otsu 11.95 Date of amendment order (Japanese: July 30, 1962) 6. Subject of amendment Application, summary 1 ``t + complete description and drawing 7, content of amendment Application μ +, purification of specification and drawings iIF (no barley history in content) Up

Claims (1)

【特許請求の範囲】 1、グリコール類寸たはその誘導体の1種あるいd、2
紳以上から選択された水溶性溶媒と水が37〜82の範
囲からなる水相成分と非イオン界面活性剤とを溶解して
界面活性剤連続相を作製し、次いで油相成分を添加せし
めて界面活性剤中油よりなるゲル状エマルンヨ/を得る
ことを特徴とするゲル状エマルンヨンの製造法。 2、グリコール類才たはその誘導体の1種あるいは21
千以上から選択された水溶性溶媒と水が3.7〜82の
範囲からなる水相成分と非イオン界面活性剤とを溶解し
て界面活性剤連続相を作製し、次いで油相成分を添加せ
しめて界面活性剤イ、1」中油よりなるゲル状エマノV
ンヨンを得た後、これに水相を添加して連続相を界面活
性剤相から水に変化させて水中油型エマルションを得る
ことを判、徴とする水中油型エマルションの製造法。
[Claims] 1. One type of glycol or its derivative or d. 2.
A surfactant continuous phase is prepared by dissolving a nonionic surfactant in a water-soluble solvent selected from a water-soluble solvent having a water content ranging from 37 to 82, and then adding an oil phase component. A method for producing a gel-like emulsion comprising obtaining a gel-like emulsion consisting of an oil in a surfactant. 2. Glycol or one of its derivatives or 21
A surfactant continuous phase is prepared by dissolving a nonionic surfactant and an aqueous phase component consisting of a water-soluble solvent selected from 1,000 or more and a water content ranging from 3.7 to 82%, and then adding an oil phase component. At least surfactant A, 1" Gel-like Emano V consisting of medium oil
A method for producing an oil-in-water emulsion, which comprises obtaining an oil-in-water emulsion by adding an aqueous phase thereto to change the continuous phase from a surfactant phase to water to obtain an oil-in-water emulsion.
JP15438182A 1982-09-05 1982-09-05 Preparation of gel like emulsion and oil in water type emulsion Granted JPS5946123A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP15438182A JPS5946123A (en) 1982-09-05 1982-09-05 Preparation of gel like emulsion and oil in water type emulsion

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP15438182A JPS5946123A (en) 1982-09-05 1982-09-05 Preparation of gel like emulsion and oil in water type emulsion

Publications (2)

Publication Number Publication Date
JPS5946123A true JPS5946123A (en) 1984-03-15
JPH0251665B2 JPH0251665B2 (en) 1990-11-08

Family

ID=15582896

Family Applications (1)

Application Number Title Priority Date Filing Date
JP15438182A Granted JPS5946123A (en) 1982-09-05 1982-09-05 Preparation of gel like emulsion and oil in water type emulsion

Country Status (1)

Country Link
JP (1) JPS5946123A (en)

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6253910A (en) * 1985-09-02 1987-03-09 Kao Corp Liquid crystal-type oily cosmetic
JPS62234540A (en) * 1985-12-23 1987-10-14 Kao Corp Gelated emulsion and o/w emulsion obtained from said emulsion
US4767625A (en) * 1985-09-02 1988-08-30 Kao Corporation Lamella type single phase liquid crystal composition and oil-base cosmetic compositions using the same
JP2001055308A (en) * 1999-06-21 2001-02-27 L'oreal Sa Organogel and use thereof in cosmetic field
KR20020007062A (en) * 2000-07-15 2002-01-26 손 경 식 Cosmetic composition of water-in-silicone emulsion type
US6346507B1 (en) 1999-03-04 2002-02-12 Shiseido Co., Ltd. Liquid crystal composition and cosmetic preparation
JP2006298788A (en) * 2005-04-18 2006-11-02 Shiseido Co Ltd Method for producing translucent cosmetics
KR20150116374A (en) * 2014-04-07 2015-10-15 한양대학교 에리카산학협력단 Method for preparing oil-in-water nanoemulsion and its use
WO2015190305A1 (en) * 2014-06-13 2015-12-17 株式会社 資生堂 Α-gel-intermediate composition, and production method for α-gel-containing o/w emulsion cosmetic using said composition
JP2016017031A (en) * 2014-07-04 2016-02-01 ロレアル Method of preparing cosmetic composition for keratin fiber
JP2017197624A (en) * 2016-04-26 2017-11-02 Jfeスチール株式会社 Flame-retardant semi-solid lubricant composition, and bearing and gear filled with the same
CN108289823A (en) * 2015-11-09 2018-07-17 花王株式会社 Composition for oral cavity
CN109199921A (en) * 2018-09-30 2019-01-15 广州启正化工科技有限公司 A kind of gel water-in-oil emulsion composition and its preparation method and application
US10231909B2 (en) 2014-06-13 2019-03-19 Shiseido Company, Ltd. α-gel-intermediate composition, and production method for α-gel-containing O/W emulsion cosmetic using said composition
EP3391872A4 (en) * 2015-12-18 2020-01-01 Pola Chemical Industries Inc. Oil-in-water type emulsion composition and method for producing same
CN111642745A (en) * 2020-06-01 2020-09-11 华中农业大学 Beta-carotene emulsion gel based on vegetable protein and nut oil and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5689832A (en) * 1979-12-24 1981-07-21 Pola Chem Ind Inc Production of oil-in-water type emulsion

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5689832A (en) * 1979-12-24 1981-07-21 Pola Chem Ind Inc Production of oil-in-water type emulsion

Cited By (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6253910A (en) * 1985-09-02 1987-03-09 Kao Corp Liquid crystal-type oily cosmetic
US4767625A (en) * 1985-09-02 1988-08-30 Kao Corporation Lamella type single phase liquid crystal composition and oil-base cosmetic compositions using the same
JPH0153845B2 (en) * 1985-09-02 1989-11-15 Kao Corp
JPS62234540A (en) * 1985-12-23 1987-10-14 Kao Corp Gelated emulsion and o/w emulsion obtained from said emulsion
JPH048104B2 (en) * 1985-12-23 1992-02-14 Kao Corp
US6346507B1 (en) 1999-03-04 2002-02-12 Shiseido Co., Ltd. Liquid crystal composition and cosmetic preparation
JP2001055308A (en) * 1999-06-21 2001-02-27 L'oreal Sa Organogel and use thereof in cosmetic field
KR20020007062A (en) * 2000-07-15 2002-01-26 손 경 식 Cosmetic composition of water-in-silicone emulsion type
JP2006298788A (en) * 2005-04-18 2006-11-02 Shiseido Co Ltd Method for producing translucent cosmetics
KR20150116374A (en) * 2014-04-07 2015-10-15 한양대학교 에리카산학협력단 Method for preparing oil-in-water nanoemulsion and its use
WO2015190305A1 (en) * 2014-06-13 2015-12-17 株式会社 資生堂 Α-gel-intermediate composition, and production method for α-gel-containing o/w emulsion cosmetic using said composition
JP2016014012A (en) * 2014-06-13 2016-01-28 株式会社 資生堂 α GEL INTERMEDIATE COMPOSITION, AND PRODUCTION METHOD OF α GEL-CONTAINING O/W EMULSION COSMETIC USING COMPOSITION THEREOF
CN106794134A (en) * 2014-06-13 2017-05-31 株式会社资生堂 The preparation method of α gels midbody composite and the O/W emulsification cosmetics containing α gels using said composition
US10231909B2 (en) 2014-06-13 2019-03-19 Shiseido Company, Ltd. α-gel-intermediate composition, and production method for α-gel-containing O/W emulsion cosmetic using said composition
US10835460B2 (en) 2014-06-13 2020-11-17 Shiseido Company, Ltd. α-Gel-intermediate composition, and production method for α-gel-containing O/W emulsion cosmetic using said composition
JP2016017031A (en) * 2014-07-04 2016-02-01 ロレアル Method of preparing cosmetic composition for keratin fiber
CN108289823A (en) * 2015-11-09 2018-07-17 花王株式会社 Composition for oral cavity
CN108289823B (en) * 2015-11-09 2021-02-26 花王株式会社 Oral composition
EP3391872A4 (en) * 2015-12-18 2020-01-01 Pola Chemical Industries Inc. Oil-in-water type emulsion composition and method for producing same
JP2017197624A (en) * 2016-04-26 2017-11-02 Jfeスチール株式会社 Flame-retardant semi-solid lubricant composition, and bearing and gear filled with the same
CN109199921A (en) * 2018-09-30 2019-01-15 广州启正化工科技有限公司 A kind of gel water-in-oil emulsion composition and its preparation method and application
CN111642745A (en) * 2020-06-01 2020-09-11 华中农业大学 Beta-carotene emulsion gel based on vegetable protein and nut oil and preparation method thereof

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