JPH0618635B2 - Water-soluble dry capsule - Google Patents
Water-soluble dry capsuleInfo
- Publication number
- JPH0618635B2 JPH0618635B2 JP60104772A JP10477285A JPH0618635B2 JP H0618635 B2 JPH0618635 B2 JP H0618635B2 JP 60104772 A JP60104772 A JP 60104772A JP 10477285 A JP10477285 A JP 10477285A JP H0618635 B2 JPH0618635 B2 JP H0618635B2
- Authority
- JP
- Japan
- Prior art keywords
- average
- capsule
- polyvinyl alcohol
- polymerization
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q13/00—Formulations or additives for perfume preparations
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/11—Encapsulated compositions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/41—Particular ingredients further characterized by their size
- A61K2800/412—Microsized, i.e. having sizes between 0.1 and 100 microns
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Veterinary Medicine (AREA)
- Organic Chemistry (AREA)
- Public Health (AREA)
- Epidemiology (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Birds (AREA)
- Cosmetics (AREA)
- Manufacturing Of Micro-Capsules (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Fats And Perfumes (AREA)
- Fertilizers (AREA)
Description
【発明の詳細な説明】 （産業上の利用分野） この発明の水溶性ドライカプセルは、水中に投下するま
ではカプセル壁内の芯物質を安全に保護し、芯物質の長
期保存を可能とすると共に芯物質の取扱いを容易にし、
カプセル壁が水と接することによりカプセル壁が溶解
し、芯物質を瞬時に放出することのできる水溶性ドライ
カプセルに係わる発明であり、芯物質として香料を内包
した場合は、風呂、洗面所等で使用する芳香剤カプセル
として利用でき、また直接手に触れることが好ましくな
く、あるいは異臭を放つような農薬、肥料等を内包して
農業、園芸用の農薬、肥料カプセルとしても利用できる
ものである。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Use) The water-soluble dry capsule of the present invention safely protects the core substance in the capsule wall until it is dropped into water, and enables long-term storage of the core substance. Together with the handling of the core substance,
It is an invention relating to a water-soluble dry capsule capable of instantly releasing a core substance by dissolving the capsule wall when the capsule wall comes into contact with water.When a perfume is included as a core substance, it is used in a bath, a washroom, etc. It can be used as a fragrance capsule to be used, or can be used as an agricultural chemical or a fertilizer capsule for agriculture or horticulture by encapsulating a pesticide, fertilizer or the like which is not preferable to be touched directly with the hands or emits an offensive odor.
（従来の技術） 従来、芯物質を壁物質で被覆した直径数ミクロンから数
百ミクロンのマイクロカプセルは、医薬、農薬、記録
材、接着剤、化粧品、香料、食品等の分野において広く
使用されており、その用途において壁物質が選定され、
特定条件下で芯物質が放出できるよう壁物質が形成され
ているものである。(Prior Art) Conventionally, microcapsules having a core substance coated with a wall substance and having a diameter of several microns to several hundreds of microns have been widely used in fields such as pharmaceuticals, agricultural chemicals, recording materials, adhesives, cosmetics, fragrances, and foods. And the wall material is selected for its use,
The wall material is formed so that the core material can be released under specific conditions.
カプセル剤の壁物質としては、無機物、有機物を問わず
広範囲に利用されており、芯物質との関係を考慮してえ
らばれ、芯物質が親油性の場合は親水性ポリマーを用
い、親水性の場合は、疎水性のポリマーが用いられるも
のである。As the wall substance of the capsule, it is widely used regardless of whether it is an inorganic substance or an organic substance, and it is selected in consideration of the relationship with the core substance.When the core substance is lipophilic, a hydrophilic polymer is used to make it hydrophilic. In some cases, hydrophobic polymers are used.
上記親水性ポリマーとしては、カゼイン、乳糖、ゼラチ
ン、アラビアゴム、澱粉、カルボキシメチルセルロー
ス、ヘキサメチルセルロース、ポリアクリル酸、ポリビ
ニルピロリドン等が用いられていた。As the hydrophilic polymer, casein, lactose, gelatin, gum arabic, starch, carboxymethyl cellulose, hexamethyl cellulose, polyacrylic acid, polyvinylpyrrolidone, etc. have been used.
しかしながら、上記親水性ポリマーは水に溶解するとは
いうものの壁膜が粗密であるため、香料等の揮発性物質
を芯物質とした場合は、いづれもカプセル保存中に壁膜
から芯物質が徐々に放出し、長期保存には耐えないもの
であり、また、異臭を放つ農薬、肥料等を芯物質とした
場合は、保存中等の取扱いにおいてはなはだ不都合なも
のであり、使用時まで芯物質を安全に保護し、芯物質の
取扱いを容易にすることが困難なものであった。However, although the hydrophilic polymer is soluble in water, since the wall film is coarse and dense, when a volatile substance such as a fragrance is used as the core substance, the core substance gradually increases from the wall film during capsule storage. It does not endure long-term storage after it is released, and when a pesticide or fertilizer that gives off an offensive odor is used as the core substance, it is very inconvenient during handling during storage, etc. It was difficult to protect and to facilitate handling of the core material.
また、壁膜を緻密に構成すれば芯物質の徐放あるいは臭
気は、ある程度防ぐことができるものの、大気中の湿気
を壁膜が吸着し易くなり、カプセルがベタついたり、極
端な場合はカプセル膜が湿気により溶解し芯物質が放出
する等し、保存管理がむつかしく、大変わずらわしいも
のであった。In addition, if the wall film is densely structured, the sustained release of the core substance or the odor can be prevented to some extent, but the wall film easily adsorbs moisture in the atmosphere, and the capsule becomes sticky or, in the extreme case, the capsule. Since the film was dissolved by moisture and the core substance was released, storage management was difficult, and it was very troublesome.
（発明の解決課題） この発明は、上記従来の水溶性カプセル壁膜の欠点に鑑
み、カプセル壁膜が水溶性であると同時に封入物をカプ
セル壁内に安全に保護し、長期保存にも耐え芯物質の取
扱いを容易にした水溶性ドライカプセルを提供するもの
である。(Problems to be Solved by the Invention) In view of the above-mentioned drawbacks of the conventional water-soluble capsule wall membrane, the present invention safely protects the encapsulated material in the capsule wall while the capsule wall membrane is water-soluble, and can withstand long-term storage. It is intended to provide a water-soluble dry capsule which facilitates the handling of a core substance.
（問題を解決するための手段） この発明は、上記課題を解決するために、結晶ブドウ糖
と結晶セルロースを吸着した疎水性物質を内包したマイ
クロカプセル壁を、平均重合度７００乃至１３００、平
均ケン化度７５％乃至９５％のポリビニルアルコールを
主剤として形成するものである。(Means for Solving the Problem) In order to solve the above problems, the present invention provides a microcapsule wall containing a hydrophobic substance adsorbing crystalline glucose and crystalline cellulose, with an average degree of polymerization of 700 to 1300 and an average saponification degree. The main component is polyvinyl alcohol having a degree of 75% to 95%.
（発明の実施例） この発明の水溶性ドライカプセルを生成するには、公知
のコアセルベーション法、液中乾燥法、液中硬化被覆
法、気中懸濁法、噴霧増粒法等のカプセル化技法を用い
ることができるものであるが、本発明の実施例における
水溶性ドライカプセルは、カプセル生成後の分離工程、
乾燥工程が同一工程で行え、装置の簡易性が計れる噴霧
増粒法によりカプセルを生成したものである。(Examples of the invention) To produce the water-soluble dry capsule of the present invention, capsules of known coacervation method, submerged drying method, submerged curing coating method, air suspension method, spray granulation method, etc. However, the water-soluble dry capsules in the examples of the present invention can be separated by a separation step after capsule formation,
The capsules are produced by the spray granulation method, which allows the drying step to be performed in the same step and the simplicity of the device to be measured.
また、芯物質としては疎水性物質である液体または固体
を問わず、水中に投下して使用する香料、農薬、肥料等
を芯物質とすることができるものであり以下の実施例、
比較例においては芯物質として香料を用いた場合につい
て示すものである。Further, as the core substance, regardless of whether it is a liquid or a solid that is a hydrophobic substance, a perfume used by dropping in water, a pesticide, a fertilizer or the like can be used as the core substance.
The comparative example shows the case where a fragrance is used as the core substance.
次に、この発明の実施例を示す。Next, examples of the present invention will be described.
実施例１ 平均重合度７５０、平均ケン化度８５％のポリビニルア
ルコール４４．３部を２５℃の水８４４．３部に加え溶
解した液に結晶ブドウ糖６．６部と結晶セルロース４．
８部を添加し攪拌した。次いでフレグランスＰＨ３１１
２（高砂香料製）１００部を上記水溶液中にミキサーで
１分間乳化し、平均粒径８．５ミクロンの水中油滴型エ
マルジョンを形成した。この乳化物を入口温度１５０
℃、出口温度９５℃、風量８ｍ3／min、アトマイザー回
転数２５０００rpmの条件下のスプレードライヤーで噴
霧乾燥し水溶性ドライカプセルを得た。Example 1 Polyvinyl alcohol (44.3 parts) having an average degree of polymerization of 750 and an average saponification degree of 85% was added to 844.3 parts of water at 25 ° C. and dissolved therein to give 6.6 parts of crystalline glucose and crystalline cellulose.
8 parts was added and stirred. Then fragrance PH311
100 parts of 2 (manufactured by Takasago) was emulsified in the above aqueous solution for 1 minute with a mixer to form an oil-in-water emulsion having an average particle size of 8.5 microns. The temperature of this emulsion is 150
° C., an outlet temperature of 95 ° C., to obtain a flow rate 8m 3 / min, spray-dried soluble dry capsules at a spray dryer under the conditions of a spray dryer 25000 rpm.
実施例２ 平均重合度９００、平均ケン化度８８％のポリビニルア
ルコール４４．３部を２５℃の水８９４．３部に加え溶
解した液に結晶ブドウ糖６．６部と結晶性セルロース
４．８部を添加し攪拌した。次に、フレグランスＰＨ−
３１１２ ５０部を上記水溶液中にミキサーで１分間乳
化し実施例１と同様に噴霧乾燥し水溶性ドライカプセル
を得た。Example 2 44.3 parts of polyvinyl alcohol having an average degree of polymerization of 900 and an average degree of saponification of 88% was added to 894.3 parts of water at 25 ° C. and dissolved to give 6.6 parts of crystalline glucose and 4.8 parts of crystalline cellulose. Was added and stirred. Next, fragrance PH-
50 parts of 3112 was emulsified in the above aqueous solution for 1 minute with a mixer and spray-dried in the same manner as in Example 1 to obtain water-soluble dry capsules.
実施例３ 実施例１の平均重合度７５０、平均ケン化度８５％のポ
リビニルアルコールの代わりに平均重合度１０００、平
均ケン化度８５％のポリビニルアルコールを使用した。Example 3 Instead of polyvinyl alcohol having an average polymerization degree of 750 and an average saponification degree of 85% in Example 1, polyvinyl alcohol having an average polymerization degree of 1000 and an average saponification degree of 85% was used.
実施例４ 実施例１の平均重合度７５０、平均ケン化度８５％のポ
リビニールアルコールの代わりに平均重合度１１００、
平均ケン化度８０％のポリビニルアルコールを使用し
た。Example 4 Instead of polyvinyl alcohol having an average degree of polymerization of 750 and an average saponification degree of 85% of Example 1, an average degree of polymerization of 1100,
Polyvinyl alcohol having an average saponification degree of 80% was used.
実施例５ 実施例１の平均重合度７５０、平均ケン化度８５％のポ
リビニルアルコールの代わりに平均重合度８００、平均
ケン化度７７％のポリビニルアルコール２２．２部と平
均重合度１７００、平均ケン化度９２％のポリビニルア
ルコール２２．２部とを使用した。Example 5 Instead of polyvinyl alcohol having an average degree of polymerization of 750 and an average saponification degree of 85% of Example 1, 22.2 parts of polyvinyl alcohol having an average degree of polymerization of 800 and an average saponification degree of 77% and an average degree of polymerization of 1700 and an average saponification degree, respectively. 22.2 parts of polyvinyl alcohol having a conversion of 92% were used.
比較例１ 実施例３の平均重合度１０００、平均ケン化度８５％の
ポリビニルアルコールの代わりにゼラチン（ニッピ−Ａ
Ｐ−１５０）を使用した。Comparative Example 1 Instead of polyvinyl alcohol having an average degree of polymerization of 1000 and an average degree of saponification of 85% of Example 3, gelatin (Nippi-A) was used.
P-150) was used.
比較例２ 実施例３の平均重合度１０００、平均ケン化度８５％の
ポリビニルアルコールの代わりにアラビアゴムＨＰ末を
使用した。Comparative Example 2 Instead of polyvinyl alcohol having an average degree of polymerization of 1000 and an average degree of saponification of 85% of Example 3, gum arabic HP powder was used.
比較例３ 実施例３の平均重合度１０００、平均ケン化度８５％の
ポリビニルアルコールの代わりにヘキサメチルセルロー
ス（和光純薬製）を使用した。Comparative Example 3 Hexamethylcellulose (manufactured by Wako Pure Chemical Industries, Ltd.) was used in place of polyvinyl alcohol having an average degree of polymerization of 1000 and an average degree of saponification of 85% in Example 3.
比較例４ 実施例３の平均重合度１０００、平均ケン化度８５％の
ポリビニルアルコールの代わりに澱粉（プルランＰＥ−
２０林原研究所製）を使用した。Comparative Example 4 Instead of polyvinyl alcohol having an average degree of polymerization of 1000 and an average degree of saponification of 85% of Example 3, starch (pullulan PE-) was used.
20 manufactured by Hayashibara Institute) was used.
比較例５ 実施例３の平均重合度１０００、平均ケン化度８５％の
ポリビニルアルコールの代わりに平均重合度５５０、平
均ケン化度８８％のポリビニルアルコールを使用した。Comparative Example 5 Instead of polyvinyl alcohol having an average degree of polymerization of 1000 and an average saponification degree of 85% in Example 3, polyvinyl alcohol having an average degree of polymerization of 550 and an average saponification degree of 88% was used.
比較例６ 実施例３の平均重合度１０００、平均ケン化度８５％の
ポリビニルアルコールの代わりに平均重合度６５０、平
均ケン化度８３％のポリビニルアルコールを使用した。Comparative Example 6 Instead of the polyvinyl alcohol having an average degree of polymerization of 1000 and an average saponification degree of 85% of Example 3, polyvinyl alcohol having an average degree of polymerization of 650 and an average saponification degree of 83% was used.
比較例７ 実施例３の平均重合度１０００、平均ケン化度８５％の
ポリビニルアルコールの代わりに平均重合度１４００、
平均ケン化度８８％のポリビニルアルコールを使用し
た。Comparative Example 7 Instead of using polyvinyl alcohol having an average degree of polymerization of 1000 and an average saponification degree of 85% in Example 3, an average degree of polymerization of 1400,
Polyvinyl alcohol having an average saponification degree of 88% was used.
比較例８ 実施例３の平均重合度１０００、平均ケン化度８５％の
ポリビニルアルコールの代わりに平均重合度１５００、
平均ケン化度８８％のポリビニルアルコールを使用し
た。Comparative Example 8 Instead of polyvinyl alcohol having an average degree of polymerization of 1000 and an average saponification degree of 85% of Example 3, an average degree of polymerization of 1500,
Polyvinyl alcohol having an average saponification degree of 88% was used.
比較例９ 実施例３の平均重合度１０００、平均ケン化度８５％の
ポリビニルアルコールの代わりに平均重合度１０００、
平均ケン化度６８．５％のポリビニルアルコールを使用
した。Comparative Example 9 Instead of the polyvinyl alcohol having an average degree of polymerization of 1000 and an average saponification degree of 85% in Example 3, an average degree of polymerization of 1000,
Polyvinyl alcohol having an average saponification degree of 68.5% was used.
比較例１０ 実施例３の平均重合度１０００、平均ケン化度８５％の
ポリビニルアルコールの代わりに平均重合度１０００、
平均ケン化度９８％のポリビニルアルコールを使用し
た。Comparative Example 10 Instead of polyvinyl alcohol having an average degree of polymerization of 1000 and an average saponification degree of 85% of Example 3, an average degree of polymerization of 1000,
Polyvinyl alcohol having an average saponification degree of 98% was used.
比較例１１ 実施例３の平均重合度１０００、平均ケン化度８５％の
ポリビニルアルコールの代わりに平均重合度１４００、
平均ケン化度９８％のポリビニルアルコールを使用し
た。Comparative Example 11 Instead of polyvinyl alcohol having an average degree of polymerization of 1000 and an average saponification degree of 85% in Example 3, an average degree of polymerization of 1400,
Polyvinyl alcohol having an average saponification degree of 98% was used.
次に、実施例１〜５および比較例１〜１１の水溶性ドラ
イカプセルの３日後、１０日後、１ケ月後における芯物
質としたフレグランスＰＨ−３１１２のカプセル内残存
率、カプセル壁の溶解時間および溶解度を第１表に示
す。Next, after 3 days, 10 days, and 1 month of the water-soluble dry capsules of Examples 1 to 5 and Comparative Examples 1 to 11, the residual rate of the fragrance PH-3112 as the core substance in the capsule, the dissolution time of the capsule wall, and The solubility is shown in Table 1.
残存率＝測定量／理論量 溶解時間＝水１００ｇに、水溶性ドライカプセル１０ｇ
を加え１０秒間攪拌。 Residual rate = measured amount / theoretical amount Dissolution time = 100 g of water, 10 g of water-soluble dry capsules
And stir for 10 seconds.
溶解度＝カプセル溶解水を濾紙で濾過後のカプセル壁残
存量 （発明の効果） 表１に示した如く、この発明による水溶性ドライカプセ
ルは、従来の水溶性ドライカプセルに比べてカプセル保
存時における芯物質の徐放が極めて少く、１ケ月後にお
いてもいづれのものも９０％以上の残存率を有するもの
であり、芯物質の保護性が極めて優れているものであ
る。さらに、カプセル使用時におけるカプセル壁の溶解
速度も極めて速く、スムースに芯物質を放出することが
でき、芯物質を有効に作用させることができるものであ
る。また、カプセル壁の溶解度も極めて高くほとんど残
存しないので、カプセルを投入した水溶液を汚損するこ
となく芯物質のみを水中で有効に利用することができる
ものである。Solubility = Amount of Capsule Wall Remaining After Filtering Dissolved Water in Capsule with Filter Paper (Effect of Invention) As shown in Table 1, the water-soluble dry capsule according to the present invention has a core at the time of storage as compared with the conventional water-soluble dry capsule. Sustained release of the substance is extremely small, and even after one month, each of them has a residual rate of 90% or more, and thus the protective property of the core substance is extremely excellent. Further, the dissolution rate of the capsule wall when the capsule is used is extremely fast, the core substance can be released smoothly, and the core substance can be effectively acted. In addition, since the solubility of the capsule wall is extremely high and hardly remains, only the core substance can be effectively used in water without contaminating the aqueous solution charged with the capsule.
フロントページの続き (51)Int.Cl.5 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｂ０１Ｊ 13/04 Ｃ０５Ｇ 5/00 Ｚ 7537−4Ｈ Continuation of the front page (51) Int.Cl. 5 Identification number Office reference number FI technical display location B01J 13/04 C05G 5/00 Z 7537-4H
Claims (1)
疎水性物質を内包したカプセル剤のカプセル壁をポリビ
ニルアルコールを主剤として形成し、該ポリビニルアル
コールは、平均重合度７００乃至１３００、平均ケン化
度７５％乃至９５％からなることを特徴とする水溶性ド
ライカプセル。1. A capsule wall of a capsule containing a hydrophobic substance adsorbing crystalline glucose and crystalline cellulose, wherein polyvinyl alcohol is used as a main component to form a capsule wall, and the polyvinyl alcohol has an average degree of polymerization of 700 to 1300 and an average degree of saponification of 75. % To 95%, a water-soluble dry capsule.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60104772A JPH0618635B2 (en) | 1985-05-16 | 1985-05-16 | Water-soluble dry capsule |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60104772A JPH0618635B2 (en) | 1985-05-16 | 1985-05-16 | Water-soluble dry capsule |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61263633A JPS61263633A (en) | 1986-11-21 |
| JPH0618635B2 true JPH0618635B2 (en) | 1994-03-16 |
Family
ID=14389767
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60104772A Expired - Fee Related JPH0618635B2 (en) | 1985-05-16 | 1985-05-16 | Water-soluble dry capsule |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0618635B2 (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02240567A (en) * | 1989-03-14 | 1990-09-25 | Sekisui Chem Co Ltd | Drug for blood taking tube and blood taking tube using this drug |
| DE4127757A1 (en) * | 1991-02-06 | 1992-08-13 | Hoechst Ag | NEW PLANT PROTECTIVE FORMULATIONS |
| JP2005509698A (en) * | 2001-11-22 | 2005-04-14 | フイルメニツヒ ソシエテ アノニム | Perfumed or flavored microcapsules containing fire retardant |
| GB0310673D0 (en) * | 2003-05-09 | 2003-06-11 | Givaudan Sa | Alginate matrix particles |
| WO2006106799A1 (en) * | 2005-03-31 | 2006-10-12 | Shionogi & Co., Ltd. | Microcapsule using polyvinyl alcohol copolymer |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2805106A1 (en) * | 1978-02-07 | 1979-08-16 | Hoechst Ag | MICROCAPSULES MADE OF POLYVINYL ALCOHOL WITH LIQUID, WATER-INSOLUBLE FILLING MATERIAL AND PROCESS FOR THEIR PRODUCTION |
| JPS58159530A (en) * | 1982-03-12 | 1983-09-21 | Nippon Synthetic Chem Ind Co Ltd:The | Formation of image |
-
1985
- 1985-05-16 JP JP60104772A patent/JPH0618635B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPS61263633A (en) | 1986-11-21 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| LAPS | Cancellation because of no payment of annual fees |