JPH05263368A - Spray-type paste composition - Google Patents

Spray-type paste composition

Info

Publication number
JPH05263368A
JPH05263368A JP5518592A JP5518592A JPH05263368A JP H05263368 A JPH05263368 A JP H05263368A JP 5518592 A JP5518592 A JP 5518592A JP 5518592 A JP5518592 A JP 5518592A JP H05263368 A JPH05263368 A JP H05263368A
Authority
JP
Japan
Prior art keywords
alkyl
spray
water
alkenyl
soluble polymer
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
JP5518592A
Other languages
Japanese (ja)
Other versions
JP3026129B2 (en
Inventor
Yoshitaka Hasegawa
美貴 長谷川
Tomoko Shibata
知子 柴田
Masaaki Yamamura
正明 山村
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.)
Kao Corp
Original Assignee
Kao Corp
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 Kao Corp filed Critical Kao Corp
Priority to JP4055185A priority Critical patent/JP3026129B2/en
Publication of JPH05263368A publication Critical patent/JPH05263368A/en
Application granted granted Critical
Publication of JP3026129B2 publication Critical patent/JP3026129B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Landscapes

  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

PURPOSE:To provide the subject composition capable of giving fabrics bulky touch, good in desizability, also causing no nozzle cloggings, essentially compris ing a water-soluble polymer paste and a long chain group-bearing specific com pound at specified proportion. CONSTITUTION:The objective composition causing no nozzle cloggings and to be used pref. by packing in a manual-type pump for domestic use comprises (A) 0.1-10wt.% of a water-soluble polymer paste (pref. hydroxyalkylated starch, CMC), (B) 0.1-5wt.% of at least one kind of compound among those of formulas I to V [R<1> and R<2> are each 12-22C alkyl, alkenyl, R<8>COOCmH2m, R<8>CONHCmH2 m, etc.; R<3>, R<4> and R<7> are each H, 1-4C alkyl, alkenyl or (CHY-CH2)nOH; R<5> and R<6> are each 11-21C alkyl, alkenyl, R<8>COO<->OCmH2m, R<9>OCOCmH2m, R<8> CONHCmH2m, R<9>NHCOCmH2m, etc. (R<8> is 11-21C alkyl, etc.; R<9> is 12-22C alkyl, etc.; (n) is 1-3; (l) is 2-3; (m) is 1-5; Q is O or NH; Y and Z are each H or methyl; X is halogen, etc.], and (C) water.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】本発明は、スプレー型糊剤組成物
に関し、詳細には衣類に対して嵩高い風合いを与えるこ
とができ、スプレーのノズルの詰りがなく、洗濯時の糊
落ちが良いスプレー型糊剤組成物に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a spray type paste composition, and more particularly, it can give a bulky texture to clothes, has no clogging of spray nozzles, and has good desizing during washing. The present invention relates to a spray type paste composition.

【0002】[0002]

【従来の技術】現在、衣料用の糊剤には、粉末、液状、
ゲル状及びスプレーの4種類のタイプがあり、各々の特
徴を生かした商品が市販されている。糊剤の内、スプレ
ー型のものは部分的にかつ手軽に使用でき便利であるた
め広く用いられている。このスプレー型の糊剤は、主に
アイロン仕上げ時に用いられ、重ね付けをすることによ
りかたさの調節を行なうことができるという利点を有す
るが、一方では、繊維の起毛を押さえ付け、布自身の厚
みを失なわさせるため、著しく風合いを損ねてしまうと
いう欠点があった。
2. Description of the Related Art Currently, sizing agents for clothing include powder, liquid,
There are four types, gel type and spray type, and products that make the most of their respective characteristics are commercially available. Of the sizing agents, the spray type is widely used because it is convenient to use partially and easily. This spray type sizing agent is mainly used at the time of ironing, and has the advantage that the hardness can be adjusted by stacking it, but on the other hand, it suppresses the raising of fibers and increases the thickness of the cloth itself. Therefore, there is a drawback that the texture is remarkably impaired.

【0003】このような欠点を改良するため、糊剤にシ
リコーンオイルのエマルジョンを配合する試みもある
が、嵩高い風合いを与える効果が十分でないばかりか、
スプレーのノズルを詰らせ、洗濯時の糊落ちも悪いとい
う問題もあった。
In order to improve such drawbacks, attempts have been made to add an emulsion of silicone oil to a sizing agent, but the effect of giving a bulky texture is not sufficient.
There was also a problem that the spray nozzle was clogged, and the paste did not come off easily during washing.

【0004】[0004]

【発明が解決しようとする課題】従って、本発明の目的
は、糊剤に求められる衣類への賦形効果はもちろんのこ
と、アイロン処理後も衣類の嵩高い風合いを保つ効果に
優れ、しかも、ノズルを詰らせることもなく、洗濯時の
糊落ちも良好なスプレー型糊剤組成物を提供することに
ある。
SUMMARY OF THE INVENTION Therefore, the object of the present invention is not only the effect of shaping a garment which is required by a sizing agent but also the effect of keeping the bulky texture of the garment after ironing, and It is an object of the present invention to provide a spray type sizing agent composition which does not clog nozzles and also has good desizing during washing.

【0005】[0005]

【課題を解決するための手段】斯かる実情に鑑み本発明
者らは鋭意研究を行なった結果、水溶性高分子糊料と特
定のジ長鎖型カチオン性化合物とを併用することによ
り、衣類への賦形効果を維持したまま、アイロンがけ後
も衣類の嵩高い風合いを保ち、かつノズルの詰りが少な
く、洗濯時の糊落ち性に優れたスプレー型糊剤組成物が
得られることを見出し本発明を完成した。
[Means for Solving the Problems] In view of such circumstances, the present inventors have conducted diligent research, and as a result, by using a water-soluble polymer paste together with a specific di-long chain type cationic compound, clothing It was found that a spray-type paste composition can be obtained which maintains the bulky texture of clothes even after ironing, has less nozzle clogging, and has excellent depigmentability during washing, while maintaining the shaping effect on The present invention has been completed.

【0006】すなわち本発明は、次の成分(a)、
(b)及び(c) (a)水溶性高分子糊料 0.1〜10重量% (b)次の一般式(1)〜(5)で表わされる化合物の1種又は2種以上 0.1〜5重量%
That is, the present invention provides the following component (a),
(B) and (c) (a) Water-soluble polymer paste 0.1 to 10% by weight (b) One or more compounds represented by the following general formulas (1) to (5). 1-5% by weight

【0007】[0007]

【化3】 [Chemical 3]

【0008】[0008]

【化4】 [Chemical 4]

【0009】(c)水を含有するスプレー型糊剤組成物
を提供するものである。
(C) A spray type paste composition containing water is provided.

【0010】本発明で用いる(a)成分の水溶性高分子
糊料としては、ヒドロキシエチル化澱粉、ヒドロキシプ
ロピル化澱粉等のヒドロキシアルキル化澱粉、カルボキ
シメチル化澱粉等のカルボキシアルキル化澱粉、及びこ
れらを過酸化水素、次亜塩素酸ナトリウム等の酸化剤又
は酵素により低粘度化したもの等の化工澱粉;カルボキ
シメチルセルロース、ポリビニルアルコール、ヒドロキ
シプロピルセルロース、ヒドロキシエチルセルロース、
メチルセルロース等のセルロース誘導体;アクリル酸、
メタクリル酸、マレイン酸、無水マレイン酸等の重合体
もしくは共重合体、又はこれらの塩;スチレンスルホン
酸重合体もしくは共重合体、又はこれらの塩等が挙げら
れるが、就中、ヒドロキシアルキル化澱粉、カルボキシ
メチルセルロース、ポリスチレンスルホン酸又はその塩
が特に好ましい。
Examples of the water-soluble polymer paste as the component (a) used in the present invention include hydroxyalkylated starches such as hydroxyethylated starch and hydroxypropylated starch, carboxyalkylated starches such as carboxymethylated starch, and the like. Modified starches such as those obtained by reducing the viscosity of hydrogen peroxide with an oxidizing agent such as sodium hypochlorite or an enzyme; carboxymethyl cellulose, polyvinyl alcohol, hydroxypropyl cellulose, hydroxyethyl cellulose,
Cellulose derivatives such as methyl cellulose; acrylic acid,
Polymers or copolymers of methacrylic acid, maleic acid, maleic anhydride, etc., or salts thereof; styrene sulfonic acid polymers or copolymers, salts thereof, etc., among which hydroxyalkylated starch is mentioned. , Carboxymethyl cellulose, polystyrene sulfonic acid or salts thereof are particularly preferable.

【0011】化工澱粉を用いる場合は、その置換度は
0.08〜0.3、特に0.1〜0.2であるものを用
いることが好ましい。置換度が0.08未満では、化工
澱粉の変性により、長期間保存すると沈澱が生成し、色
ものの衣類に使用した時に白化現象がより激しくなる。
また、化工澱粉の置換度が0.3より大きいものを用い
た場合、張り強度の低下傾向が認められるため好ましく
ない。化工澱粉の水溶液の粘度は、過酸化水素、次亜塩
素酸ナトリウムなどの酸化剤又は酵素で化工澱粉を分解
することにより低下可能であり、例えば5重量%(以下
「%」で示す)水溶液では40センチポイズ(以下cpと
する)(20℃)以下の粘度が良く、これ以上の粘度で
はスプレー性が良好でなく、その結果白化現象が起こり
やすくなる。
When the modified starch is used, it is preferable that the substitution degree thereof is 0.08 to 0.3, particularly 0.1 to 0.2. If the degree of substitution is less than 0.08, the modified starch will be modified to form a precipitate when stored for a long period of time, and the whitening phenomenon will become more intense when used for colored clothes.
Further, when a modified starch having a degree of substitution of more than 0.3 is used, the tensile strength tends to decrease, which is not preferable. The viscosity of an aqueous solution of modified starch can be reduced by decomposing the modified starch with an oxidizing agent such as hydrogen peroxide, sodium hypochlorite, or an enzyme. For example, in an aqueous solution of 5% by weight (hereinafter referred to as “%”), Viscosity of 40 centipoise (hereinafter referred to as cp) (20 ° C.) or lower is good, and if the viscosity is higher than this, the sprayability is not good, and as a result, the whitening phenomenon easily occurs.

【0012】また、カルボキシメチルセルロースを用い
る場合、そのエーテル化度は、0.6〜1.5、特に
0.8〜1.0の範囲のものが好ましく、その1%水溶
液の粘度が100cp以下、特に50cp以下のものが好ま
しい。更に前記のアクリル酸等又はスチレンスルホン酸
等の重合体又は共重合体は、その分子量が1万〜120
万、特に5万〜60万の範囲のものが好ましい。 (a)成分の配合量は、全組成物中0.1〜10%、特
に0.3〜5%とするのが好ましい。
When carboxymethyl cellulose is used, its etherification degree is preferably in the range of 0.6 to 1.5, particularly 0.8 to 1.0, and its 1% aqueous solution has a viscosity of 100 cp or less, Particularly, those having 50 cp or less are preferable. Further, the above-mentioned polymers or copolymers of acrylic acid or styrene sulfonic acid have a molecular weight of 10,000 to 120.
It is preferably in the range of 10,000, particularly in the range of 50,000 to 600,000. The compounding amount of the component (a) is preferably 0.1 to 10%, and more preferably 0.3 to 5% in the total composition.

【0013】本発明で用いる(b)成分は、前記一般式
(1)〜(5)で表わされるものであるが、就中、炭素
数16〜22の長鎖基を2本有し、かつ少なくとも1本
はエステル基又はアミド基で連結されている長鎖基を有
する化合物が好適に使用される。なお、これらの2本の
長鎖基はそれぞれ炭素数が異なっていてもよい。 (b)成分は、本発明のスプレー型糊剤組成物中0.1
〜5%、特に0.1〜1%配合することが好ましい。
The component (b) used in the present invention is represented by the above general formulas (1) to (5), and in particular, it has two long chain groups having 16 to 22 carbon atoms, and A compound having at least one long-chain group linked by an ester group or an amide group is preferably used. The two long-chain groups may have different carbon numbers. The component (b) is 0.1 in the spray type paste composition of the present invention.
It is preferable to add -5%, especially 0.1-1%.

【0014】本発明のスプレー型糊剤組成物には、上記
必須成分の他、更に必要に応じてクエン酸、リンゴ酸、
安息香酸、酒石酸等の有機酸、ポリエチレングリコー
ル、グリセリン、ポリプロピレングリコールの如きアイ
ロン付着防止剤、エチルアルコール、プロピルアルコー
ル、プロピレングリコール等の溶剤、蛍光染料、抗菌
剤、殺菌剤、香料、缶腐食防止剤等を添加することがで
きる。
In addition to the above essential components, the spray-type paste composition of the present invention may further contain citric acid, malic acid,
Organic acids such as benzoic acid and tartaric acid, iron adhesion inhibitors such as polyethylene glycol, glycerin and polypropylene glycol, solvents such as ethyl alcohol, propyl alcohol and propylene glycol, fluorescent dyes, antibacterial agents, bactericides, fragrances and can corrosion inhibitors Etc. can be added.

【0015】本発明のスプレー型糊剤組成物はポンプ式
或いはトリガー式のスプレー容器に充填し使用しても良
く、またエアゾール用の耐圧罐に噴射剤と共に充填し使
用することもできる。エアゾール用の場合、用いる噴射
剤としては液化プロパン、液化ブタン、及びそれらの混
合物、或いはジメチルエーテルを使用するのが良い。噴
射剤と本発明の組成物との重量比率は噴射剤:本発明組
成物=3:97〜40:60が好ましく、更に好ましく
は5:95〜30:70である。なお、エアゾール型糊
剤を充填した缶は、糊料水溶液のため缶の腐食、倒立又
は横向き使用によるエアゾールスプレーの噴射ガス欠乏
等の問題があり、また缶は、使い捨てであり、資源の有
効利用が図れない。更にエアゾール式の場合高圧ガスを
用いるため、家庭用には不向きな場合がある。従って、
高圧ガスを使用しないポンプ式又はトリガー式が有利で
あるが、従来の糊剤を用いるとノズルが詰りやすいとい
う欠点がある。しかしながら本発明の糊剤組成物は、ノ
ズルが詰りにくいという特徴を有するため、このような
手動式のスプレーにも好適に使用することができる。
The spray type paste composition of the present invention may be used by filling it in a pump type or trigger type spray container, or by filling it with a propellant in a pressure can for an aerosol. In the case of an aerosol, it is preferable to use liquefied propane, liquefied butane, and a mixture thereof, or dimethyl ether as a propellant to be used. The weight ratio of the propellant to the composition of the present invention is preferably propellant: composition of the present invention = 3: 97 to 40:60, more preferably 5:95 to 30:70. In addition, the can filled with the aerosol type sizing agent has problems such as corrosion of the sizing agent due to the aqueous solution of sizing agent, lack of injection gas of the aerosol spray due to upside down or sideways use, and the can is disposable and effective use of resources Cannot be achieved. Further, since the aerosol type uses high-pressure gas, it may not be suitable for home use. Therefore,
A pump type or a trigger type that does not use high-pressure gas is advantageous, but using a conventional sizing agent has a drawback that the nozzle is easily clogged. However, since the sizing agent composition of the present invention has a feature that the nozzle is unlikely to be clogged, it can be suitably used for such a manual spray.

【0016】[0016]

【発明の効果】本発明のスプレー型糊剤組成物は、衣類
に嵩高い風合いを与えることができ、スプレーのノズル
の詰りがなく、洗濯時の糊落ち性が良い。
EFFECTS OF THE INVENTION The spray-type paste composition of the present invention can give a bulky texture to clothes, has no clogging of the spray nozzle, and has good desmearability during washing.

【0017】[0017]

【実施例】以下、実施例を挙げて本発明を更に詳細に説
明するが、本発明はこれらに限定されるものではない。 実施例1 水溶性高分子糊料として、No.6(表1)の組成物以
外のもの(表1、表2)には、置換度0.11〜0.1
3、粘度3〜8cp(10%水溶液、25℃)のヒドロキ
シプロピル澱粉を2.0%用い、No.6のものは平均
分子量150,000のポリスチレンスルホン酸ナトリ
ウム2.0%を用い、これと表1、表2に示す化合物
0.5%とを組み合せ、残部は水を加え、糊剤組成物を
調製した。これを手動式ポンプ(トリガー)容器に充填
し、ポリエステル/木綿(65/35 ブロード60
番)混紡布に100%o.w.f(of weight
ofFabric)になるよう噴霧後、アイロンの指
示温度(木綿の目盛に合わせた)でアイロンがけを行な
った。
The present invention will be described in more detail with reference to examples, but the present invention is not limited thereto. Example 1 As a water-soluble polymer paste, no. 6 (Table 1) other than the composition (Table 1, Table 2), the substitution degree of 0.11 to 0.1
No. 3, using 2.0% of hydroxypropyl starch having a viscosity of 3 to 8 cp (10% aqueous solution, 25 ° C.), No. For No. 6, 2.0% sodium polystyrene sulfonate having an average molecular weight of 150,000 was used, and this was combined with 0.5% of the compounds shown in Tables 1 and 2, and water was added to the balance to prepare a paste composition. Prepared. Fill this into a manual pump (trigger) container and use polyester / cotton (65/35 broad 60
No.) 100% o. w. f (of weight
After spraying so as to be of Fabric, ironing was performed at the indicated temperature of the iron (matched to the scale of cotton).

【0018】この後、布を20℃、65%相対湿度の恒
温恒湿室に一昼夜放置し、嵩高性の試験を行なった。嵩
高性試験は10名のパネラーによる官能試験によった。
すなわち、嵩高さを−2から2の5段階で評価し、その
人数を表1、表2に示した。
After that, the cloth was left to stand in a constant temperature and constant humidity chamber at 20 ° C. and 65% relative humidity for a whole day and night, and a bulkiness test was conducted. The bulkiness test was performed by a sensory test by 10 panelists.
That is, the bulkiness was evaluated on a scale of -2 to 2, and the number of persons was shown in Tables 1 and 2.

【0019】[0019]

【表1】 [Table 1]

【0020】[0020]

【表2】 [Table 2]

【0021】ノズルの詰り試験:No.1,4,6,
7,8をトリガー容器に300ml充填したサンプルを夫
々50本を作った。30℃の恒温室に入れ1週間毎に各
サンプルをとり出し振とうし、5秒間噴射し、再度保存
を続ける。10回繰返した(10週間)後、つまりの状
態を観察した。完全につまった、或いは噴射状態不良の
本数はNo.1は2本、No.4は1本、No.6は0
本、No.7は0本、No.8は10本であった。 糊落ち性試験:No.1,4,8をトリガー容器に充填
し、ポリエステル/木綿混紡布(65/35)に100
%o.w.fになるように噴霧後、アイロン指示温度
(木綿の目盛に合わせた)でアイロンがけをした。この
糊付けした布をターゴトメーター型洗濯試験機で洗剤
(市販品、花王(株)製、アタック)の0.0833%
洗浄液で洗濯(20℃、15分間)し、次いで5分間す
すぎ、脱水、風乾、アイロンがけした。上記糊付けと洗
濯を3回繰り返した後、張り硬さを、JIS1005−
1959に準拠してカンチレバー法により測定した。未
処理の布は4.2、No.1は4.5、No.4は4.
3、No.8は6.0であり、本発明品は優れた糊落ち
性を示した。
Nozzle clogging test: No. 1, 4, 6,
50 samples were made by filling the trigger container with 300 ml of 7 and 8, respectively. Put in a thermostatic chamber at 30 ° C., take out each sample every week, shake, spray for 5 seconds, and continue storage again. After repeating 10 times (10 weeks), the clogged state was observed. The number of completely clogged or defective injection states is No. 1 is 2 pieces, No. 1 No. 4 is one, 6 is 0
Book No. No. 7 is No. 8 was 10. Glue removal test: No. Fill 1, 4 and 8 into a trigger container and add 100 to polyester / cotton blended fabric (65/35)
% O. w. After spraying to reach f, ironing was performed at the ironing temperature (matched to the scale of cotton). 0.0833% of the detergent (commercially available product, manufactured by Kao Corporation, Attack) with a tergotometer-type washing tester on this glued cloth
It was washed with the washing solution (20 ° C., 15 minutes), then rinsed for 5 minutes, dehydrated, air-dried and ironed. After repeating the above-mentioned gluing and washing three times, the tensile hardness was measured according to JIS1005-
According to 1959, it measured by the cantilever method. Untreated cloth is 4.2, No. No. 1 is 4.5, No. 1 4 is 4.
3, No. No. 8 was 6.0, and the product of the present invention showed excellent desmearability.

───────────────────────────────────────────────────── 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 7199−3B D06M 21/00 Z ─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 5 Identification code Office reference number FI technical display location 7199-3B D06M 21/00 Z

Claims (1)

【特許請求の範囲】[Claims] 【請求項1】 次の成分(a)、(b)及び(c) (a)水溶性高分子糊料 0.1〜10重量% (b)次の一般式(1)〜(5)で表わされる化合物の1種又は2種以上 0.1〜5重量% 【化1】 【化2】 (c)水を含有するスプレー型糊剤組成物。1. The following components (a), (b) and (c) (a) Water-soluble polymer paste 0.1 to 10% by weight (b) The following general formulas (1) to (5) One or more of the compounds represented 0.1-5% by weight [Chemical 2] (C) A spray-type paste composition containing water.
JP4055185A 1992-03-13 1992-03-13 Spray type paste composition Expired - Fee Related JP3026129B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP4055185A JP3026129B2 (en) 1992-03-13 1992-03-13 Spray type paste composition

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP4055185A JP3026129B2 (en) 1992-03-13 1992-03-13 Spray type paste composition

Publications (2)

Publication Number Publication Date
JPH05263368A true JPH05263368A (en) 1993-10-12
JP3026129B2 JP3026129B2 (en) 2000-03-27

Family

ID=12991658

Family Applications (1)

Application Number Title Priority Date Filing Date
JP4055185A Expired - Fee Related JP3026129B2 (en) 1992-03-13 1992-03-13 Spray type paste composition

Country Status (1)

Country Link
JP (1) JP3026129B2 (en)

Also Published As

Publication number Publication date
JP3026129B2 (en) 2000-03-27

Similar Documents

Publication Publication Date Title
GB2302877A (en) Aerosol ironing aid comprising non-polysaccharide stiffening agent and dimethyl ether
JPH05263368A (en) Spray-type paste composition
JP3184378B2 (en) Finishing composition for clothing
JPH05239774A (en) Finishing agent for clothing
EP0364887A2 (en) High hydrocarbon tolerant hair fixing compositions having superior shampoo removability
JP3886582B2 (en) Antifouling composition and method for treating textile products
JPH09241973A (en) Sizing agent composition for spray
JP4275236B2 (en) Textile treatment agent
JPS591819B2 (en) Spray-glue composition
JPH0559672A (en) Spray-type sizing agent composition
JP3207021B2 (en) Sizing composition and spray type sizing article
JP2575844B2 (en) Spray type paste composition
JPH02112477A (en) Spray type sizing agent composition
JPH01153796A (en) Detergent composition
JPS593590B2 (en) Spray type glue composition
JPS593585B2 (en) Aerosol glue composition
JP3805399B2 (en) Spray paste composition
GB1589482A (en) Fabric stiffening composition
JP2584571B2 (en) Spray type paste composition
JPH11229266A (en) Spray type sizing agent composition
JP2946143B2 (en) Spray type paste composition
JP3100781B2 (en) Liquid soft finish
JP2986600B2 (en) Spray type paste composition
JP4514851B2 (en) Glue
JP2989709B2 (en) Liquid soft finish

Legal Events

Date Code Title Description
R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

FPAY Renewal fee payment (prs date is renewal date of database)

Year of fee payment: 9

Free format text: PAYMENT UNTIL: 20090128

FPAY Renewal fee payment (prs date is renewal date of database)

Year of fee payment: 9

Free format text: PAYMENT UNTIL: 20090128

FPAY Renewal fee payment (prs date is renewal date of database)

Free format text: PAYMENT UNTIL: 20100128

Year of fee payment: 10

LAPS Cancellation because of no payment of annual fees