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JP5032022B2 - Method for producing foamable oil and fat composition - Google Patents
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JP5032022B2 - Method for producing foamable oil and fat composition - Google Patents

Method for producing foamable oil and fat composition Download PDF

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JP5032022B2
JP5032022B2 JP2005350653A JP2005350653A JP5032022B2 JP 5032022 B2 JP5032022 B2 JP 5032022B2 JP 2005350653 A JP2005350653 A JP 2005350653A JP 2005350653 A JP2005350653 A JP 2005350653A JP 5032022 B2 JP5032022 B2 JP 5032022B2
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oil
fat composition
fat
foamable
composition
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JP2007153796A (en
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裕之 加藤
嘉彦 高瀬
政続 山下
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Taiyo Kagaku Co Ltd
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for producing a stable foaming oil and fat composition having persistency. <P>SOLUTION: The above problem is solved by including a step for confirming existence of needle crystals having &le;1 &mu;m diameter and 2-200 &mu;m length in oil and fat. <P>COPYRIGHT: (C)2007,JPO&amp;INPIT

Description

本発明は、油脂中で針状結晶の存在を確認する工程を有する起泡性油脂組成物の製造方法に関する。   The present invention relates to a method for producing a foamable oil / fat composition having a step of confirming the presence of needle-like crystals in the oil / fat.

従来、起泡性油脂組成物の調製は、研究者の経験と勘に頼ることが多く、必ずしも目的の起泡性油脂を手にいれることができずにいた。さらに起泡性油脂組成物になり得るか、良好な泡質であるかどうかは、実際にポンプフォーマーやエアゾール形態にして起泡性を確認するしかなく工程中で簡単に判断する製法は無かった。日本工業規格には、一般的な水系に於ける泡の評価法が記されているが、油系における泡については起泡性が低く、評価しにくいという欠点があった。(例えば非特許文献1参照。)   Conventionally, the preparation of a foamable oil / fat composition often relies on the experience and intuition of researchers, and the desired foamable oil / fat cannot always be obtained. Whether it can be a foamable oil or fat composition or has good foam quality, there is no production method that can be easily judged in the process without actually checking the foamability in the form of a pump former or aerosol. It was. Japanese Industrial Standards describe a method for evaluating foam in a general aqueous system, but foam in an oil system has a drawback that foaming is low and evaluation is difficult. (For example, refer nonpatent literature 1.)

JIS K 3362法JIS K 3362 method

持続性のある安定な起泡性油脂組成物の製造方法を提供することを目的とする。   It aims at providing the manufacturing method of the stable and foamable oil-fat composition which is durable.

界面活性剤及び界面活性剤と油脂からなる特定形状(直径1μm以下、長さ2〜200μm)の針状結晶を含有することにより上記課題を解決する。   The above-mentioned problems are solved by containing a surfactant and a needle-shaped crystal having a specific shape (diameter: 1 μm or less, length: 2-200 μm) composed of a surfactant and an oil and fat.

本発明の針状結晶とは、界面活性剤及び界面活性剤と油脂からなる微細針状結晶を表し、針状結晶の生成には特定の油脂と界面活性剤が適量含まれる溶液を調製することで得ることができる。調製された起泡性油脂組成物はポンプフォーマー及びエアゾール形態にて充填し噴射することで起泡性油脂を得ることができる。針状結晶の数、大きさの測定方法としては、特に限定されるものではないが、例えば80℃にて溶液を調製したものをスライドガラスに0.1ml滴下し25℃2時間冷却後、常温常圧にてスケール付ノルマルスキー型位相差顕微鏡を使用し200μm四方の視野中にて観察する方法が挙げられる。起泡性油脂組成物の良好な泡沫生成及び安定化を得るためには、針状結晶が100μm四方に1から100個存在することが好ましく、より好ましくは30〜80個、さらに好ましくは70〜80個が望ましい。大きさとして直径1μm以下、長さ2〜200μmが好ましく、より好ましくは直径1μm以下、長さ10〜100μmであり、さらに好ましくは直径1μm以下、長さ30〜50μmが望ましい。   The acicular crystals of the present invention represent surfactants and fine acicular crystals composed of a surfactant and an oil and fat, and a solution containing appropriate amounts of specific oils and surfactants is prepared for the formation of acicular crystals. Can be obtained at The prepared foamable oil / fat composition can be obtained by filling and injecting in the form of a pump former and an aerosol and then spraying. The method for measuring the number and size of needle crystals is not particularly limited. For example, 0.1 ml of a solution prepared at 80 ° C. is dropped on a slide glass and cooled at 25 ° C. for 2 hours, and then at room temperature. There is a method of observing in a 200 μm square visual field using a normalsky type phase contrast microscope with a scale at normal pressure. In order to obtain good foam generation and stabilization of the foamable oil and fat composition, it is preferable that 1 to 100 acicular crystals exist in a 100 μm square, more preferably 30 to 80, and even more preferably 70 to 80 is desirable. The size is preferably 1 μm or less in diameter and 2 to 200 μm in length, more preferably 1 μm or less in diameter and 10 to 100 μm in length, and further preferably 1 μm or less in diameter and 30 to 50 μm in length.

本発明は従来、研究者の経験と勘に頼るしか方法が無かった起泡性油脂組成物の起泡性の評価が、実際に起泡試験をすることを必要とせず、油脂組成物の結晶観察を行うことにより評価できる製造方法及び評価方法を提供するものである。   In the present invention, the evaluation of foamability of a foamable oil and fat composition, which conventionally had no way to rely on the experience and intuition of a researcher, did not actually require a foaming test. A manufacturing method and an evaluation method that can be evaluated by observation are provided.

本発明で用いられる油脂としては、起泡時に液状のものであれば、特に限定するものではなく、天産品でも化学合成品でもよい。例えばアボガド油、ツバキ油、タートル油、マカダミアナッツ油、トウモロコシ油、ミンク油、オリーブ油、ナタネ油、卵黄油、ごま油、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、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状油脂、流動パラフィン、スクワレン、スクワラン、プリスタン等の炭化水素、オレイン酸、トール油、イソステアリン酸等の高級アルコール脂肪酸、ラウリルアルコール、オレイルアルコール、イソステアリルアルコール、オクチルドデカノール等の高級アルコール、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、デカメチルポリシロキサン等のシリコーン、ミリスチン酸イソプロピル、パルミチン酸イソプロピル、ラウリン酸ヘキシル、オレイン酸オレイル、オレイン酸デシルミリスチン酸オクチルドデシル、ジメチルオクタン酸ヘキシルデシル、フタル酸ジエチル、フタル酸ジブチル等のエステル類等が挙げられる。また、上記油脂に水素添加、分別等の処理を施して得られるものでもよい。なお、グリセリド成分としての不飽和脂肪酸、側鎖状脂肪酸やジグリセリド、モノグリセリド等は若干量であれば含まれていてもかまわない。   The oil and fat used in the present invention is not particularly limited as long as it is liquid at the time of foaming, and may be a natural product or a chemically synthesized product. For example, 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, Cotton oil, eno oil, soybean oil, peanut oil, tea seed oil, kaya oil, rice bran oil, cinnagiri oil, Japanese kiri oil, jojoba oil, germ oil, trioctanoic acid glycerin, triisopalmitic acid glycerin and other liquid oils and liquid paraffin , Hydrocarbons such as squalene, squalane and pristane, higher alcohol fatty acids such as oleic acid, tall oil, isostearic acid, higher alcohols such as lauryl alcohol, oleyl alcohol, isostearyl alcohol, octyldodecanol, methyl polysiloxane, methyl phenyl poly Siloxane, methyl high Silicone such as rhogen polysiloxane and decamethylpolysiloxane, isopropyl myristate, isopropyl palmitate, hexyl laurate, oleyl oleate, decyl oleate octyldodecyl myristate, hexyldecyl dimethyloctanoate, diethyl phthalate, dibutyl phthalate Ester etc. are mentioned. Moreover, what is obtained by processing the said fats and oils, such as hydrogenation and fractionation, may be used. It should be noted that unsaturated fatty acids, side chain fatty acids, diglycerides, monoglycerides and the like as glyceride components may be contained in a slight amount.

本発明で用いられる油脂の配合量は、特に限定するものではないが、好ましくは、起泡性油脂組成物全量中の10〜99重量%であり、さらに好ましくは30〜95重量%である。   Although the compounding quantity of the fats and oils used by this invention is not specifically limited, Preferably, it is 10 to 99 weight% in the whole foamable fat and oil composition, More preferably, it is 30 to 95 weight%.

また、本発明で用いられる界面活性剤としては、グリセリン脂肪酸エステルであれば、特に限定されるものではないが、例えば、モノカプリン、モノカプリリン、モノラウリン、モノミリスチン、モノパルミチン、モノオレイン、モノステアリン、モノべへニンが望ましい。   The surfactant used in the present invention is not particularly limited as long as it is a glycerin fatty acid ester. For example, monocaprin, monocaprylin, monolaurin, monomyristin, monopalmitin, monoolein, monostearin, Monobehenine is desirable.

グリセリン脂肪酸エステルの配合量は、特に限定するものではないが、好ましくは起泡性油脂組成物の油脂分に対して0.01〜50重量%であり、より好ましくは0.1〜30重量%であり、さらに好ましくは1〜20重量%である。   The blending amount of the glycerin fatty acid ester is not particularly limited, but is preferably 0.01 to 50% by weight, more preferably 0.1 to 30% by weight, based on the fat and oil content of the foamable fat and oil composition. More preferably, it is 1 to 20% by weight.

本発明の起泡性油脂組成物は、さらに噴射剤を添加してエアゾールタイプとしてもよい。   The foamable oil and fat composition of the present invention may be an aerosol type by further adding a propellant.

本発明に用いられる噴射剤は、特に限定されるものではないが例えばトリクロロフルオロメタン、ジクロロジフルオロメタン、ジクロロフルオロメタン、トリクロロトリフルオロメタン、ジクロロテトラフルオロメタン等のクロロフルオロカーボン、プロパン、イソブタン、イソペンタン、ノルマルブタン及び液化石油ガス(以下LPGと略す)等の液化ガスであり、泡質及び泡沫安定性の点から好ましくはプロパン、イソブタン、イソペンタン、ノルマルブタン、LPGであり、より好ましくはLPGである。これらの噴射剤に加えてジメチルエーテル、炭酸ガス、窒素ガスを用いても良い。これらのガスは単独でもまた2種類以上を混合しても用いることができる。配合量は組成物の2〜90重量%が好ましい。2重量%未満では良好な泡沫が得にくく、90重量%より多いと泡沫が飛散し扱いづらい。   The propellant used in the present invention is not particularly limited, but for example, chlorofluorocarbons such as trichlorofluoromethane, dichlorodifluoromethane, dichlorofluoromethane, trichlorotrifluoromethane, dichlorotetrafluoromethane, propane, isobutane, isopentane, norma It is a liquefied gas such as rubane and liquefied petroleum gas (hereinafter abbreviated as LPG), and is preferably propane, isobutane, isopentane, normal butane, or LPG, more preferably LPG from the viewpoint of foam quality and foam stability. In addition to these propellants, dimethyl ether, carbon dioxide gas, or nitrogen gas may be used. These gases can be used alone or in combination of two or more. The blending amount is preferably 2 to 90% by weight of the composition. If it is less than 2% by weight, it is difficult to obtain a good foam, and if it exceeds 90% by weight, the foam is scattered and difficult to handle.

本発明のエアゾールとは、容器中に起泡性油脂組成物と噴射剤を充填して得られるものである。本発明は、上記に挙げた噴射剤を配合しても良いが、噴射剤を配合せずに空気の吹き込み混合による、いわゆるノンガスタイプでも泡沫化が可能である。   The aerosol of the present invention is obtained by filling a foamable oil and fat composition and a propellant in a container. In the present invention, the above-mentioned propellant may be blended, but foaming is possible even in a so-called non-gas type by blowing and mixing air without blending the propellant.

本発明の針状結晶を含有する起泡性油脂組成物の製造方法には、上記の必須成分の他に本発明の目的を達成する範囲で他の成分を適宜配合することができる。例えば、ポリグリセリン脂肪酸エステル、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、ポリオキシエチレンアルキルエーテル、ポリオキシプロピレンアルキルエーテル、ポリオキシエチレンアルキルフェニルエーテル、ポリオキシエチレングリコール脂肪酸エステル、ポリオキシエチレンアルキルエーテル、アルキロールアマイド、ポリオキシエチレン硬化ヒマシ油等の界面活性剤、ポリオキシエチレン・メチルポリシロキサン共重合体、ポリオキシエチレン・ポリオキシプロピレンメチルポリシロキサン共重合体等のポリエーテル変性シリコーンオイル、アルキルリン酸、アルキルエーテルリン酸等のリン酸エステル、酸化チタン、タルク、ベントサイト、カチオン、マイカ等の粉末、防腐剤、色剤、酸化防止剤、水、香料、薬剤、固型油分、半固型油分、アルコール、保湿剤等が挙げられる。   In the method for producing a foamable oil and fat composition containing acicular crystals of the present invention, in addition to the above-mentioned essential components, other components can be appropriately blended within the scope of achieving the object of the present invention. For example, polyglycerin fatty acid ester, sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene alkyl ether, polyoxypropylene alkyl ether, polyoxyethylene alkyl phenyl ether, polyoxyethylene glycol fatty acid ester, polyoxyethylene alkyl ether, Surfactant such as alkylol amide, polyoxyethylene hydrogenated castor oil, polyether-modified silicone oil such as polyoxyethylene / methylpolysiloxane copolymer, polyoxyethylene / polyoxypropylenemethylpolysiloxane copolymer, alkyl phosphorus Acids, phosphoric acid esters such as alkyl ether phosphoric acid, titanium oxide, talc, bentsite, cations, mica powders, preservatives, colorants, oxidation Sealant, water, perfume, drug, solid oil component, semisolid oil component, an alcohol, humectants, and the like.

本発明の起泡性油脂組成物の用途としては、特に限定するものではないが、油汚れ等の洗浄剤、口紅、ファンデーションなどの化粧料のクレンジング剤、日焼け用オイル、ベビーオイル、ヘアーオイル、泡状マッサージオイル等が挙げられ、好ましくは、ベビーオイルとしての用途がよい。   The use of the foamable oil and fat composition of the present invention is not particularly limited, but is a cleaning agent such as oil stains, a cleansing agent for cosmetics such as lipstick and foundation, suntan oil, baby oil, hair oil, Foamed massage oils and the like can be mentioned, and the use as baby oil is preferable.

次に実施例によって本発明を更に詳細に説明する。なお、本発明はこれらの実施例に限定されるものではない。   Next, the present invention will be described in more detail by way of examples. The present invention is not limited to these examples.

実施例1 ベビーオイル用起泡性油脂組成物
表1に示した原料配合に基づき、以下の方法で、保湿タイプの起泡性油脂組成物を調製した。
Example 1 Foamable oil / fat composition for baby oil Based on the raw material formulation shown in Table 1, a moisturizing type foamable oil / fat composition was prepared by the following method.

表1の原料1から10までを80℃にて攪拌溶解し、常温まで冷却することで、保湿タイプの起泡性油脂組成物を得た。その後、100mlエアゾール缶に組成物18gを充填し、バルブをセットし、噴射剤として液化石油ガス2gを充填し、上記起泡性油脂組成物を得た。得られた起泡性油脂組成物を本発明品A〜Lとした。また表1の原料1から10までを80℃溶解して得た起泡性油脂組成物0.1mlをスライドに滴下し、25℃2時間冷却したものを顕微鏡観察用試料とした。※表中の原料名における( )内の数字は、酸化エチレンの付加モル数を示す。以下、同じ。   The raw materials 1 to 10 in Table 1 were stirred and dissolved at 80 ° C. and cooled to room temperature to obtain a moisturizing type foamable oil and fat composition. Thereafter, 18 g of the composition was filled in a 100 ml aerosol can, a valve was set, and 2 g of liquefied petroleum gas was filled as a propellant to obtain the foamable oil and fat composition. The obtained foamable oil-fat composition was made into this invention product AL. Further, 0.1 ml of a foamable oil / fat composition obtained by dissolving raw materials 1 to 10 in Table 1 at 80 ° C. was dropped on a slide and cooled at 25 ° C. for 2 hours to obtain a sample for microscope observation. * The numbers in parentheses in the raw material names in the table indicate the number of moles of ethylene oxide added. same as below.

Figure 0005032022
Figure 0005032022

比較例1 ベビーオイル用起泡性油脂組成物
表2に示した原料配合に基づき、実施例1と同様にして、保湿タイプの起泡性油脂組成物を調製した。
Comparative Example 1 Foamable oil / fat composition for baby oil A moisturizing type foamable oil / fat composition was prepared in the same manner as in Example 1 based on the raw material composition shown in Table 2.

すなわち、本発明品A〜Fに対し、界面活性剤未配合の同油性成分配合組成物を比較品A、ポリオキシエチレン(2)セチルエーテル配合の同油性成分配合組成物を比較品B、デカグリセリンモノオレイン酸エステル配合の同油性成分配合組成物を比較品C、テトラグリセリンモノステアリン酸エステル配合の同油性成分配合組成物を比較品D、ポリオキシエチレン(2)オレイルエーテルとポリオキシエチレン(4)ラウリルエーテルリン酸ナトリウム配合の同油性成分配合組成物を比較品Eとして、実施例1と同様の方法で上記起泡性油脂組成物を得た。   That is, for the products A to F of the present invention, the same oily component blending composition containing no surfactant is used as a comparative product A, and the same oily component blending composition containing a polyoxyethylene (2) cetyl ether is used as a comparison product B. The oil-based component blended composition containing glycerin monooleate ester is Comparative Product C, the oil-based component blended composition blended with tetraglycerin monostearate ester is Comparative Product D, polyoxyethylene (2) oleyl ether and polyoxyethylene ( 4) The said foamable oil-fat composition was obtained by the method similar to Example 1 by making the same oil-based component mixing | blending composition containing sodium lauryl ether phosphate into the comparative product E.

Figure 0005032022
Figure 0005032022

試験例1
本発明品A〜Lと、比較品A〜Eを比較した。
評価方法および評価基準は以下の通りである。
Test example 1
The inventive products A to L and the comparative products A to E were compared.
Evaluation methods and evaluation criteria are as follows.

(泡形成状態)
泡形成状態は肉眼観察にて行った。評価基準は極めて均一できめ細かい泡を◎、均一できめ細かい泡を〇、きめが粗い泡を△、泡にならず液状を×とした。各エアゾールをアクリル板(縦:10cm、横:10cm)上に噴射した直後に判定した。
(泡安定性)
形成した泡の持続性を評価した。評価基準は泡が持続するものを○とし崩壊までの時間を記し、全く泡とならず液状であるものを×とした。
(針状結晶の数、大きさの確認)
マイクロメーター付ノルマルスキー型位相差顕微鏡を用い、常温常圧にて起泡性油脂組成物の針状結晶の数、大きさを評価した。針状結晶があるものは○としその数を明記し、無いものは×とした。また針状結晶の直径と長さを測定した。
結果を表3に示す。
(Bubble formation state)
Foam formation was performed by visual observation. The evaluation criteria were extremely uniform and fine bubbles ◎, uniform and fine bubbles ◯, coarsely textured bubbles Δ, and liquid that did not become bubbles X. Each aerosol was judged immediately after being sprayed onto an acrylic plate (length: 10 cm, width: 10 cm).
(Foam stability)
The persistence of the foam formed was evaluated. As the evaluation criteria, a case where bubbles persisted was marked as ◯, a time until collapse was recorded, and a case where bubbles were not formed at all and was in a liquid state was marked as x.
(Check the number and size of needle crystals)
The number and size of the needle-like crystals of the foamable oil and fat composition were evaluated at normal temperature and pressure using a normalsky phase contrast microscope with a micrometer. Those with needle-like crystals were marked with ◯, the number was specified, and those without needles were marked with x. The diameter and length of the needle-like crystals were measured.
The results are shown in Table 3.

Figure 0005032022
Figure 0005032022

表3に示すように、本発明品A〜Lは針状結晶を含有し、使用性に優れ、且つ、きめの細かい泡沫、泡沫持続安定性も良好であるのに対し、比較品A〜Eは全く泡にならなかった。以上のように油脂組成物中の針状結晶とその起泡性の間には、高い相関関係があることが判明した。このため、従来行われていた開発者の経験と勘に頼る方法とは異なり、予め油脂組成物の針状結晶を観察することにより、起泡性を評価する方法を見出した。   As shown in Table 3, the products A to L of the present invention contain needle-like crystals, are excellent in usability, and have fine fine bubbles and good foam stability, while comparative products A to E. Did not foam at all. As described above, it has been found that there is a high correlation between the needle-like crystal in the oil and fat composition and its foamability. For this reason, the method of evaluating foaming property by observing the needle-like crystal | crystallization of an oil-fat composition previously was found unlike the method based on the experience and intuition of the developer performed conventionally.

Claims (3)

グリセリン脂肪酸エステルと油脂を含有する油脂組成物であって、油脂中で直径1μm以下、長さ2〜200μmの大きさである針状結晶の存在を確認する工程を有することを特徴とする起泡性油脂組成物の製造方法。   A foam composition comprising a glycerin fatty acid ester and an oil and fat, comprising a step of confirming the presence of needle-like crystals having a diameter of 1 μm or less and a length of 2 to 200 μm in the oil or fat. Method for producing an oily fat composition. グリセリン脂肪酸エステルと油脂を含有する油脂組成物中で直径1μm以下、長さ2〜200μmの大きさである針状結晶の存在を確認することを特徴とする油脂組成物の起泡性評価方法。   A method for evaluating foamability of an oil or fat composition, wherein the presence of needle-like crystals having a diameter of 1 μm or less and a length of 2 to 200 μm in an oil or fat composition containing a glycerin fatty acid ester and an oil or fat is confirmed. グリセリン脂肪酸エステルと油脂を含有する油脂組成物中で直径1μm以下、長さ2〜200μmの大きさである針状結晶を含有することを特徴とする起泡性油脂組成物。   A foamable oil and fat composition comprising needle-like crystals having a diameter of 1 μm or less and a length of 2 to 200 μm in an oil and fat composition containing a glycerin fatty acid ester and an oil and fat.
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