JPH02274258A - Manufacture of water-containing arginic acid film - Google Patents

Manufacture of water-containing arginic acid film

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Publication number
JPH02274258A
JPH02274258A JP1096123A JP9612389A JPH02274258A JP H02274258 A JPH02274258 A JP H02274258A JP 1096123 A JP1096123 A JP 1096123A JP 9612389 A JP9612389 A JP 9612389A JP H02274258 A JPH02274258 A JP H02274258A
Authority
JP
Japan
Prior art keywords
film
aqueous solution
soluble
alginate
calcium salt
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
JP1096123A
Other languages
Japanese (ja)
Other versions
JP2940930B2 (en
Inventor
Kunio Yoneto
邦夫 米戸
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.)
Sekisui Chemical Co Ltd
Original Assignee
Sekisui Chemical Co Ltd
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Priority to JP1096123A priority Critical patent/JP2940930B2/en
Publication of JPH02274258A publication Critical patent/JPH02274258A/en
Application granted granted Critical
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Expired - Lifetime legal-status Critical Current

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  • Materials For Medical Uses (AREA)
  • Cosmetics (AREA)

Abstract

PURPOSE:To enable easy continuous manufacture having no dispersion of effective components by forming a film of a soluble arginic salt aqueous solution, spraying a soluble calcium salt aqueous solution to this film, and gelling the film of said aqueous solution, and forming a gelled film. CONSTITUTION:An arginic acid salt is dissolved in water to form an aqueous solution. This solution is adjusted to have a viscosity within the range of several hundreds to several ten thousands cps so that a film can be formed by general coating method. Separately to this, an aqueous solution of soluble calcium salt is prepared. This is adjusted in such a manner that the quantity of the contained calcium ion is preferably 0.2 to 0.35 moles per mole of Na ion contained in the sodium arginate aqueous solution. The concentration of the soluble calcium salt aqueous solution is preferably 1 to 20wt.%. Then the soluble arginate aqueous solution is spread on a base film to form a film, to which the soluble calcium salt aqueous solution is sprayed. Gelling occurs simultaneously with spraying, so that the water-containing arginic film can be continuously produced at high efficiency.

Description

【発明の詳細な説明】 (産業上の利用分野) 本発明は、医薬品や化粧品等の外用剤として利用される
、含水アルギン酸フィルムの製造方法に関する。
DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a method for producing a hydrous alginic acid film that is used as an external preparation for pharmaceuticals, cosmetics, and the like.

(従来の技術) 可m 性アルギン酸塩は、水溶液中でカルシウムイオン
等の2価金属塩と反応すると、容易にゲル化することが
知られている。この性質を利用して、含水アルギン酸フ
ィルムを製造することができる。
(Prior Art) It is known that flexible alginates easily gel when reacted with divalent metal salts such as calcium ions in an aqueous solution. Utilizing this property, a hydrous alginic acid film can be produced.

含水アルギン酸フィルムは、医薬品、化粧品等の外用剤
に応用され得る。これらの外用剤は、その用途に応じて
薬効成分、保湿剤、殺菌剤、着色剤等の有効成分及びそ
の他の添加剤を含有する。このような含水アルギン酸フ
ィルムは、一般に、上記有効成分を含む可溶性アルギン
酸塩水溶液を、ゲル化することにより得られる。
The hydrated alginic acid film can be applied to external preparations such as pharmaceuticals and cosmetics. These external preparations contain active ingredients such as medicinal ingredients, humectants, bactericidal agents, colorants, and other additives depending on their intended use. Such a hydrous alginate film is generally obtained by gelling a soluble alginate aqueous solution containing the above-mentioned active ingredient.

含水アルギン酸フィルムの具体的な製造方法としては、
例えば英国特許第552,770号に、アルギン酸ナト
リウム(以下、アルギン酸Naとする)水溶液を、塩化
カルシウム水溶液等の溶液(ゲル化溶液)中に押し出す
方法が開示されている。ゲル化溶液中に押し出されたア
ルギン酸Naは、カルシウムイオンと反応して即座にゲ
ル化し、含水アルギン酸フィルムを形成する。しかしこ
の方法では、アルギン酸Na水溶液中に薬効成分、保湿
剤等が配合されている場合には、該有効成分が、形成さ
れたゲル状物(含水アルギン酸フィルム)から上記ゲル
化溶液中へ溶出するため、得られる含水アルギン酸フィ
ルム中の有効成分の含有量が一定しない。そのため、上
記方法は、医薬品や化粧品用の外用剤の製造には適して
いない。
The specific method for producing a hydrous alginate film is as follows:
For example, British Patent No. 552,770 discloses a method in which an aqueous solution of sodium alginate (hereinafter referred to as Na alginate) is extruded into a solution (gelling solution) such as an aqueous calcium chloride solution. The Na alginate extruded into the gelling solution reacts with calcium ions and immediately gels to form a hydrous alginic acid film. However, in this method, when medicinal ingredients, humectants, etc. are blended into the Na alginate aqueous solution, the active ingredients are eluted from the formed gel (hydrated alginate film) into the gelling solution. Therefore, the content of the active ingredient in the obtained hydrated alginic acid film is not constant. Therefore, the above method is not suitable for producing external preparations for pharmaceuticals and cosmetics.

含水アルギン酸フィルムの他の製造方法が、食品工業、
Vol、10.No、4.  (1967)に記載され
ている。この文献に記載された方法に於ては、アルギン
酸Na水溶液に難溶性カルシウム塩を添加し、これを製
膜、放置することによりゲル化が達成される。この方法
では、難溶性のカルシウム塩を使用するため、アルギン
酸Na水溶液中に形成されるカルシウムイオンの濃度は
非常に低い。従って、アルギン酸Naとカルシウムイオ
ンとの反応が遅くなり、その結果、ゲル化前にこの溶液
を流延し製膜することが可能となる。しかし、この方法
において、カルシウム塩のmを調節するなどの手段によ
り、ゲル化速度を遅くすると、この溶液を流延後ゲル化
するまでの間、長時間放置しなければならないので、連
続製造の効率が低下してしまう。逆にゲル化速度を速く
すると、この溶液を流延し製膜する前にゲル化してしま
う。
Other methods for producing hydrated alginate films are used in the food industry,
Vol, 10. No, 4. (1967). In the method described in this document, gelation is achieved by adding a sparingly soluble calcium salt to an aqueous solution of Na alginate, forming a film, and leaving it to stand. In this method, since a poorly soluble calcium salt is used, the concentration of calcium ions formed in the Na alginate aqueous solution is very low. Therefore, the reaction between Na alginate and calcium ions is slowed down, and as a result, it becomes possible to cast this solution to form a film before gelation. However, in this method, if the gelation rate is slowed down by means such as adjusting the m of the calcium salt, the solution must be left for a long time after casting until it gels, which makes continuous production difficult. Efficiency will decrease. On the other hand, if the gelation rate is increased, the solution will gel before being cast to form a film.

言い換えれば、上記方法は製造条件の設定が難く、連続
製造には適していない。
In other words, the above method is difficult to set manufacturing conditions and is not suitable for continuous manufacturing.

(発明が解決しようとする課題) 本発明は上記従来の問題点を解決するものであり、その
目的は、有効成分のバラツキがなく、容易に連続製造す
ることができ、医薬品や化粧品の分野の外用剤を得るの
に好適な含水アルギン酸フィルムの製造方法を提供する
ことである。
(Problems to be Solved by the Invention) The present invention solves the above-mentioned conventional problems.The purpose of the present invention is to have no variation in active ingredients, easy continuous production, and to be useful in the fields of pharmaceuticals and cosmetics. An object of the present invention is to provide a method for producing a hydrous alginic acid film suitable for obtaining an external preparation.

(課題を解決するための手段) 本発明の含水アルギン酸フィルムの製造方法は、可溶性
アルギン酸塩水溶液の膜を形成する工程と、該水溶液の
膜に可溶性カルシウム塩水溶液を噴霧して、該水溶液の
膜をゲル化しゲル状のフィルムを得る工程と、を包含し
ており、そのことによって上記目的が達成される。
(Means for Solving the Problems) The method for producing a hydrous alginate film of the present invention includes the steps of forming a film of a soluble alginate aqueous solution, and spraying a soluble calcium salt aqueous solution onto the film of the aqueous solution. and a step of gelling the gel to obtain a gel-like film, thereby achieving the above object.

本発明に用いられる可溶性アルギン酸塩は、アルギン酸
のL i 、K s N a等のアルカリ金属塩である
The soluble alginates used in the present invention are alkali metal salts of alginic acid, such as L i and K s Na.

本発明に用いられる可溶性カルシウム塩としては、ハロ
ゲン化カルシウム(フッ化カルシウムを除く)、硝酸カ
ルシウム、及び酢酸カルシウムを挙げることができる。
Soluble calcium salts used in the present invention include calcium halides (excluding calcium fluoride), calcium nitrate, and calcium acetate.

本発明の含水アルギン酸フィルムには、必要に応じて各
種の有効成分や添加剤が含有され得る。
The hydrous alginic acid film of the present invention may contain various active ingredients and additives as necessary.

その例としては、各種の薬効成分、保湿剤、殺菌剤、抗
菌剤、着色剤、増粘剤、薬効成分の吸収促進剤、中和・
緩衝剤、着味料、香料、界面活性剤、軟化剤、有機・無
機増量剤等がある。
Examples include various medicinal ingredients, humectants, bactericidal agents, antibacterial agents, colorants, thickeners, absorption enhancers for medicinal ingredients, neutralizers,
These include buffering agents, flavorings, fragrances, surfactants, softeners, organic and inorganic fillers, etc.

本発明の含水アルギン酸フィルムを調製するには、まず
、上記アルギン酸塩を水に溶解させ、水溶液とする。こ
の水溶液は、通常の塗工方式で製膜し得るように、数百
〜敵方cpsの粘度の範囲に調整される。この範囲より
低粘度或いは高粘度では、製膜が困難となり、好ましく
ない。
To prepare the hydrated alginic acid film of the present invention, first, the above alginate is dissolved in water to form an aqueous solution. This aqueous solution is adjusted to have a viscosity in the range of several hundred cps so that it can be formed into a film using a normal coating method. If the viscosity is lower or higher than this range, it becomes difficult to form a film, which is not preferable.

次に、これとは別に、上記可溶性カルシウム塩の水溶液
を調製する。可溶性カルシウム塩水溶液は、含有される
カルシウムイオンの量が、上記アルギン酸Na水溶液に
含有されるNaイオン1モルあたり、0.15〜0.4
モル、好ましくは02〜0.35モルとなるように調製
される。この範囲よりも多いと、得られる含水アルギン
酸フィルムは固くなり、例えば医療用の貼付剤とすると
、使用感が悪くなる。この範囲よりも少ないと、殆どゲ
ル化が起こらず、フィルムの強度が小さくなる。可溶性
カルシウム塩水溶液の濃度は、通常、1〜50重量%、
好ましくは1〜20重量%である。この範囲より高い濃
度の水溶液を用いると、該水溶液が噴霧されたアルギン
酸塩水溶液の膜が収縮し、得られるフィルムに変形が生
じると共に離水現象が生じる。この範囲よりも低い濃度
ではゲル化速度が遅くなり、また、噴霧する水溶1ff
iが多くなることにより、有効成分の溶出の可能性が出
てくる。
Next, separately, an aqueous solution of the above-mentioned soluble calcium salt is prepared. The soluble calcium salt aqueous solution contains 0.15 to 0.4 calcium ions per mole of Na ions contained in the above Na alginate aqueous solution.
mol, preferably 02 to 0.35 mol. If the amount exceeds this range, the obtained hydrated alginic acid film becomes hard, and when used as a medical patch, for example, the feeling of use becomes poor. When the amount is less than this range, gelation hardly occurs and the strength of the film decreases. The concentration of the soluble calcium salt aqueous solution is usually 1 to 50% by weight,
Preferably it is 1 to 20% by weight. If an aqueous solution with a concentration higher than this range is used, the film of the alginate aqueous solution onto which the aqueous solution is sprayed will shrink, deforming the resulting film and causing a water separation phenomenon. If the concentration is lower than this range, the gelation rate will be slow, and the aqueous solution 1ff to be sprayed will be
As i increases, the possibility of elution of the active ingredient increases.

次に、上記可溶性アルギン酸塩水溶液を常法、例えばキ
ャスティング法により、基材フィルム、例えばポリエチ
レンテレフタレートフィルム上に流延して製膜し、これ
に対して、上記可溶性カルシウム塩水溶液が噴霧される
。噴霧された可溶性カルシウム塩水溶液中のカルシウム
イオンは、速やかにアルギン酸塩と反応するので、ゲル
化は噴霧と同時に起こる。そのため、含水アルギン酸フ
ィルムを効率的に連続製造することができる。生成した
含水アルギン酸フィルムは、必要に応じて基材フィルム
から剥離して使用される。調製された含水アルギン酸フ
ィルムの厚みは、使用目的により異なるが、通常Q、1
mm〜5mmである。このフィルムは、従来技術の項で
記した英国特許の方法のように、含水アルギン酸フィル
ムが溶液中に形成されることがないので、有効成分や必
要とされる添加剤が失われない。得られた含水アルギン
酸フィルムは、必要に応じて延伸処理される。このこと
によりフィルムの強度、透明度等が同上する。
Next, the soluble alginate aqueous solution is cast onto a base film, eg, a polyethylene terephthalate film, to form a film by a conventional method, such as a casting method, and the soluble calcium salt aqueous solution is sprayed onto the film. Calcium ions in the sprayed soluble calcium salt aqueous solution quickly react with the alginate, so that gelation occurs simultaneously with spraying. Therefore, a hydrous alginic acid film can be efficiently and continuously produced. The produced hydrous alginic acid film is peeled off from the base film and used, if necessary. The thickness of the prepared hydrous alginate film varies depending on the purpose of use, but is usually Q, 1
mm to 5 mm. This film does not result in the formation of a hydrous alginate film in the solution, as in the British patent process described in the prior art section, so that active ingredients and required additives are not lost. The obtained hydrous alginic acid film is subjected to stretching treatment, if necessary. This improves the strength, transparency, etc. of the film.

(実施例) 本発明を実施例について以下に説明する。(Example) The invention will now be described with reference to examples.

支籠匠上 アルギン酸Na(君津化学工業型、Isグレード)2重
量部を、日本薬局方精製水98重量部に均一に溶解した
。この水溶液をポリエチレンテレフタレートフィルム上
に、厚み1mmに流延した。
Two parts by weight of Shikago Takumi Na alginate (Kimitsu Chemical Industry type, Is grade) were uniformly dissolved in 98 parts by weight of Japanese Pharmacopoeia purified water. This aqueous solution was cast onto a polyethylene terephthalate film to a thickness of 1 mm.

この上から、塩化カルシウム(牛丼化学製、試薬特級)
水溶液を、表1に示す濃度で噴霧した。噴霧されるカル
シウムイオンの全量は、何れの場合も一定であり、アル
ギン酸Na水溶液に含有されるNaイオン1モルに対し
て0. 2モルである。
From above, calcium chloride (made by Gyudon Kagaku, reagent special grade)
Aqueous solutions were sprayed at the concentrations shown in Table 1. The total amount of calcium ions to be sprayed is constant in all cases, and is 0.000% per mole of Na ions contained in the Na alginate aqueous solution. It is 2 moles.

塩化カルシウム水溶液を噴霧後、2分間放置し、得られ
た含水アルギン酸フィルムの性状を観察した。その結果
も併せて表1に示す。
After spraying the calcium chloride aqueous solution, it was left to stand for 2 minutes, and the properties of the resulting hydrated alginic acid film were observed. The results are also shown in Table 1.

(以下余白) 表  1 表1から、塩化カルシウム水溶液の好ましい濃度は、1
〜50重量%であり、更に好ましい濃度は1〜20重ユ
%であることが明らかである。
(Margin below) Table 1 From Table 1, the preferred concentration of the calcium chloride aqueous solution is 1
It is clear that the concentration is 50% by weight, and a more preferred concentration is 1 to 20% by weight.

X籠匠主 アルギン酸Na(君津化学工業型、Isグレード)2重
量部を、日本薬局方精製水98重量部に均一に溶解した
。この水溶液をポリエチレンテレフタレートフィルム上
に、厚み1IllI11に流延した。
2 parts by weight of X-Kagoshosho Na alginate (Kimitsu Chemical Industry type, Is grade) was uniformly dissolved in 98 parts by weight of Japanese Pharmacopoeia purified water. This aqueous solution was cast onto a polyethylene terephthalate film to a thickness of 1IllI11.

この上から、5重量%塩化カルシウム(牛丼化学製、試
薬特級)水溶液を噴霧した。ここで噴霧されるカルシウ
ムイオンの全量は、アルギン酸Na水溶液に含有される
Naイオン1モルに対して、表2に示す量となるように
、上記水溶液が噴霧された。塩化カルシウム水溶液を噴
霧後、2分間放置し、得られた含水アルギン酸フィルム
の強度及び使用感を調べた。その結果も併せて表2に示
す。
A 5% by weight calcium chloride aqueous solution (manufactured by Gyudon Kagaku, reagent grade) was sprayed onto this. The aqueous solution was sprayed in such a manner that the total amount of calcium ions sprayed was as shown in Table 2 per 1 mole of Na ions contained in the aqueous solution of Na alginate. After spraying an aqueous calcium chloride solution, the film was allowed to stand for 2 minutes, and the strength and feel of the resulting hydrated alginic acid film were examined. The results are also shown in Table 2.

ここで、フィルムの強度及び使用感は、官能試験により
調べられた。
Here, the strength and usability of the film were examined through a sensory test.

(以下余白) ψ噴霧面に離水現象が見られる。(Margin below) ψA syneresis phenomenon is observed on the spray surface.

表 *アルギン酸Na水溶液に含有されるNaイオン1モル
に対するカルシウムイオンのモル数表2から、噴霧され
るカルシウムイオンの好ましい量は、アルギン酸Naに
含有されるNa1モルに対して、0゜15〜0.4モル
であり、更に好ましい量は、0.2〜0.35モルであ
ることが明らかである。
Table * Number of moles of calcium ions per mole of Na ions contained in the Na alginate aqueous solution From Table 2, the preferred amount of calcium ions to be sprayed is 0°15 to 0 per mole of Na contained in the Na alginate solution. It is clear that the preferred amount is between 0.2 and 0.35 mol.

裏ム匹エ アルギン酸Na(君津化学工業製、ISグレード)2重
量部と、銅クロロフィリンNa0.01重量部とを、日
本薬局方精製水97.99重皿部に均一に溶解した。こ
の水溶液をポリエチレンテレフタレートフィルム上に、
厚み2mmに流延した。
2 parts by weight of Na alginate (manufactured by Kimitsu Chemical Industries, IS grade) and 0.01 part by weight of copper chlorophyllin Na were uniformly dissolved in 97.99 parts by weight of Japanese Pharmacopoeia purified water. This aqueous solution was placed on a polyethylene terephthalate film.
It was cast to a thickness of 2 mm.

この上から、5重1%塩化カルシウム(牛丼化学製試薬
特級)水溶液を噴霧した。ここで噴霧されるカルシウム
イオンの全量は、アルギン酸Na水溶液に含有されるN
aイオン1モルに対して0゜2モルである。塩化カルシ
ウム水溶液を噴霧後、2分間放置した。得られた含水ア
ルギン酸フィルム中の銅クロロフィリンNaの含有ヱは
、フィルム形成前のそれとほぼ等しかった。フィルムの
強度及び使用感は共に良好であった。
A 5-fold 1% calcium chloride aqueous solution (special grade reagent manufactured by Gyudon Kagaku) was sprayed on top of this. The total amount of calcium ions sprayed here is the amount of N contained in the Na alginate aqueous solution.
The amount is 0.2 mol per 1 mol of a ions. After spraying the calcium chloride aqueous solution, it was left for 2 minutes. The content of copper chlorophyllin Na in the obtained hydrated alginic acid film was almost equal to that before film formation. The strength and usability of the film were both good.

実JLfL± 実施例3で得られた含水アルギン酸フィルムを、フィル
ム延伸装置を用いて、50 g / cmで延伸処理し
た。延伸処理したフィルムは、延伸処理しないフィルム
と比較して、フィルム強度が大きく、遜明性が良好であ
った。
Actual JLfL± The hydrous alginate film obtained in Example 3 was stretched at 50 g/cm using a film stretching device. The stretched film had greater film strength and better clarity than the unstretched film.

(発明の効果) 本発明の製造方法によれば、このように、含有される有
効成分のバラツキのない含水アルギン酸フィルムが、効
率良く連続製造され得る。本発明方法を適用すれば、医
薬品、化粧品等の分野で使用されるアルギン酸を基剤と
する外用剤を、一定品質で、効率よく、連続的に製造し
得る。
(Effects of the Invention) According to the production method of the present invention, a water-containing alginic acid film without variation in the contained active ingredients can be efficiently and continuously produced in this way. By applying the method of the present invention, alginic acid-based external preparations used in the fields of pharmaceuticals, cosmetics, etc. can be efficiently and continuously manufactured with constant quality.

以上that's all

Claims (1)

【特許請求の範囲】 1、可溶性アルギン酸塩水溶液の膜を形成する工程と、 該水溶液の膜に可溶性カルシウム塩水溶液を噴霧して、
該水溶液の膜をゲル化しゲル状のフィルムを得る工程と
、 を包含する含水アルギン酸フィルムの製造方法。 2、前記ゲル状のフィルムをさらに延伸処理する工程を
包含する請求項1に記載の含水アルギン酸フィルムの製
造方法。
[Claims] 1. Forming a film of a soluble alginate aqueous solution, and spraying a soluble calcium salt aqueous solution onto the film of the aqueous solution,
A method for producing a water-containing alginic acid film, comprising: gelling a film of the aqueous solution to obtain a gel-like film. 2. The method for producing a hydrous alginic acid film according to claim 1, which includes the step of further stretching the gel-like film.
JP1096123A 1989-04-14 1989-04-14 Method for producing hydrous alginate film Expired - Lifetime JP2940930B2 (en)

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US20100144909A1 (en) * 2007-01-22 2010-06-10 Hideaki Ichiura Method for producing functional material, functional material, sheet-like structure and sanitary product

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JP3073154U (en) * 2000-05-10 2000-11-14 ティー・ミナミ株式会社 Decorative light set

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JPS6218082A (en) * 1985-07-16 1987-01-27 Sharp Corp Semiconductor laser device

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Publication number Priority date Publication date Assignee Title
JP3073154U (en) * 2000-05-10 2000-11-14 ティー・ミナミ株式会社 Decorative light set

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100144909A1 (en) * 2007-01-22 2010-06-10 Hideaki Ichiura Method for producing functional material, functional material, sheet-like structure and sanitary product
US8440731B2 (en) * 2007-01-22 2013-05-14 Unicharm Corporation Method for producing functional material, functional material, sheet-like structure and sanitary product
US9101911B2 (en) * 2007-01-22 2015-08-11 Unicharm Corporation Method for producing functional material, functional material, sheet-like structure and sanitary product

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