JP3862873B2 - Textile treatment composition - Google Patents

Textile treatment composition Download PDF

Info

Publication number
JP3862873B2
JP3862873B2 JP29952398A JP29952398A JP3862873B2 JP 3862873 B2 JP3862873 B2 JP 3862873B2 JP 29952398 A JP29952398 A JP 29952398A JP 29952398 A JP29952398 A JP 29952398A JP 3862873 B2 JP3862873 B2 JP 3862873B2
Authority
JP
Japan
Prior art keywords
water
weight
average molecular
molecular weight
soluble
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
Application number
JP29952398A
Other languages
Japanese (ja)
Other versions
JP2000129577A (en
Inventor
靖 吉田
信之 小倉
宗郎 青柳
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 JP29952398A priority Critical patent/JP3862873B2/en
Publication of JP2000129577A publication Critical patent/JP2000129577A/en
Application granted granted Critical
Publication of JP3862873B2 publication Critical patent/JP3862873B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Landscapes

  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Description

【0001】
【発明の属する技術分野】
本発明は繊維製品処理剤組成物に関する。
【0002】
【従来の技術及び発明が解決しようとする課題】
現在、家庭で着用された衣料の洗濯には通常弱アルカリ性重質洗剤が使用されており、また、おしゃれ着等の洗濯には軽質洗剤が使用されている。また、これらの衣料は好みによって、衣料を柔らかく仕上げる柔軟剤や硬く仕上げる糊料が使用されている。
【0003】
しかしながら衣料の洗浄を繰り返すと、繊維の傷みによる襟や袖口の縮みが生じ、また張りがなくなり見た目や着心地が悪くなる。また、このような衣料を柔軟剤や糊剤で処理を行うと衣料の形がくずれたり、本来の風合いを損なう等の問題があった。
【0004】
従って、本発明の目的は衣料本来の形状と風合いを回復させる処理剤を提供することである。
【0005】
【課題を解決するための手段】
本発明は、(A)重量平均分子量5000〜500000の水溶性加工澱粉及びその誘導体並びに重量平均分子量10000〜500000の水溶性セルロース誘導体からなる群から選ばれる水溶性高分子化合物0.1〜20重量%、(B)シリコーン化合物0.5〜5重量%及び(C)非イオン性界面活性剤0.1〜5重量%を含有する繊維製品処理剤組成物に関する。
【0006】
【発明の実施の形態】
(A)成分の水溶性加工澱粉の重量平均分子量は、5000〜500000、好ましくは10000〜500000である。水溶性加工澱粉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、カルボキシメチル化澱粉、第4級アンモニウム基を有するカチオン化澱粉又はこれらを酸化剤(例えばH22、NaClO等)又は酵素により低粘度化したものが好ましい。この場合において、澱粉に対してヒドロキシエチル基、カルボキシメチル基や4級アンモニウム基等の置換基が導入される割合を示す置換度(澱粉の全水酸基数に対する置換基が導入されている水酸基数の割合)は、保存安定性と風合い付与の点で、好ましくは0.08〜0.8、より好ましくは0.1〜0.4である。
【0007】
また、(A)成分の水溶性セルロース誘導体としては、ヒドロキシメチルセルロース、ヒドロキシエチルセルロース、ヒドロキシプロピルセルロース等のヒドロキシアルキルセルロース、メチルセルロース、エチルセルロース等のアルキルセルロース、カルボキシメチルセルロース、4級アンモニウム基を有するカチオン化セルロース等を挙げることができ、重量平均分子量が10000〜500000、好ましくは50000〜200000のものが用いられる。これらの置換度は0.5〜1.5、好ましくは0.6〜1.0である。
【0008】
これら水溶性高分子化合物(A)の重量平均分子量は、ポリエチレングリコールを標準物質とするゲルパーミエーションクロマトグラフィー法により測定されたものである。
【0009】
また、本発明において、水溶性高分子化合物とは、80℃の水100gに対し水溶性高分子化合物1gを加えたときにその液が濁らずに澄明になるものをいう。
【0010】
(B)成分のシリコーン化合物としては、ジ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、アミノ変性シリコーン、アミド変性シリコーン、エポキシ変性シリコーン、カルボキシ変性シリコーン、ポリエーテル変性シリコーン等を挙げることができ、特にジメチルポリシロキサン、アミノ変性シリコーン、ポリエーテル変性シリコーンが良好である。シリコーン化合物の重量平均分子量は1000〜1000000、好ましくは2000〜100000である。シリコーン化合物の重量平均分子量は、分子量が既知のジメチルポリシロキサンを基準にゲルパーミエーションクロマトグラフィー法により求めることができる。また、シリコーン化合物は粒子が分散した水性エマルジョンの形態で配合することが好ましく、分散粒子の平均粒径は0.01〜10μm、特に0.01〜0.5μm、更には0.05〜0.1μmが良好である。
【0011】
(C)成分の非イオン性界面活性剤としては、ポリオキシアルキレンアルキル又はアルケニルエーテル、ポリオキシアルキレンアルキルフェニルエーテル、ポリオキシアルキレンソルビタン脂肪酸エステル、ポリオキシアルキレングリコール脂肪酸エステル、ポリオキシエチレンポリオキシプロピレンブロックポリマー等が挙げられる。特にポリオキシエチレンアルキル又はアルケニル(炭素数10〜20)エーテル型非イオン性界面活性剤が好ましい。これらはグリフィン法によるHLBが12〜18のものが好ましい。特に好ましい(C)成分としては、下記一般式(I)の化合物を例示することができる。
R−(OC24)n−OH (I)
〔式中、Rは炭素数12〜20のアルキル基又はアルケニル基、nは5〜30の数であり、RとnはHLBが12〜18の範囲になるように調整される。〕
本発明の繊維製品処理剤組成物は、良好な衣料の形態回復効果と風合い付与効果が得られることから、(A)成分を0.1〜20重量%、好ましくは1〜15重量%含有する。また、貯蔵安定性と形態回復効果が良好である点で、(B)成分を0.5〜5重量%、好ましくは0.5〜3重量%、更に(C)成分を0.1〜5重量%、好ましくは0.3〜3重量%含有する。
【0012】
本発明の繊維製品処理剤組成物には、通常の柔軟剤や糊剤に使用されている成分を配合しても差し支えない。このような成分としては陽イオン性界面活性剤、陰イオン性界面活性剤、香料、色素、抗菌剤、エチレングリコール、プロピレングリコール等の溶媒、食塩、塩化アンモニウム、塩化カルシウム等の無機塩等が挙げられる。
【0013】
本発明の繊維製品処理剤組成物は、上記(A)〜(C)成分及び任意成分を含有し、通常、残部は水である。また、本発明の組成物は、適度な濃度に希釈して使用される。例えば、衣料を通常の洗濯を行い、すすぎの段階ですすぎ水に本発明の組成物を溶解させて処理を行ったり、また、たらいのような容器を用い本発明の組成物を水に溶解させ、更に衣料を入れてを浸漬処理する方法が考えられる。繊維製品の処理は何れの方法で行っても良いが、(A)成分の処理浴中の濃度が10ppm〜1000ppm、特に20ppm〜500ppmとなるようにするのが好ましく、浴比(衣料に対する処理液の比率)は1/3〜1/100、特に1/5〜1/50が好ましい。
【0014】
【実施例】
<繊維製品処理剤組成物の調製>
表1に示した組成物を調製した。なお、各成分については以下の通りである。
【0015】
・カチオン化セルロース A−1
(置換度1.7〜2.2、重量平均分子量150000)
・カチオン化澱粉 A−2
(置換度0.2〜0.3、重量平均分子量100000)
・酢酸ビニル−メタクリル酸共重合体水分散エマルション A−3
(有効分40%、水不溶性高分子)
・シリコーン B−1
〔東レ・ダウコーニング・シリコーン(株)製、SM8705、平均粒径0.03〜0.04μm、重量平均分子量80000〕
・ジタローイルジメチルアンモニウムクロライド B−2
・非イオン性界面活性剤 C−1
〔ポリオキシエチレン(平均付加モル数20)アルキル(炭素数12)エーテル、HLB16.8〕
・プロピレングリコール D−1
なお、A−1及びA−2の水への溶解度は、1g/100g(80℃)以上であり、澄明性を示した。また、A−3の水への溶解度は、0.01g/100g(80℃)未満であり、エマルションであった。
【0016】
<被処理繊維製品の調製>
青色の木綿100%のポロシャツを5枚用意し、4枚をナショナル製洗濯機NA−F60Eを用い、市販の重質洗剤を用いて20回繰り返し洗濯処理をした。これら4枚の衣料の襟、袖口は張りがなく、繊維が伸びたような形状がみられ、新品から見るとかなり劣化している。
【0017】
<処理方法>
5Lのたらいに水5Lを入れ、表1の組成物20gを溶解させた(A−1又はA−2濃度400ppm、浴比=1/30)。上記の洗濯処理したポロシャツの1枚を10分間浸漬させ、その後洗濯機で脱水し、陰干しをした。
【0018】
<評価基準>
訓練された評価者により、上記で用いたポロシャツの新品と上記処理を行ったポロシャツの形態を比較し、以下の基準で判定した。結果を表1に併せて示した。
新品と同等の形態にまで回復した;+2
新品までは回復しないが、満足できるレベルまで回復した;+1
未処理品と同等であった;0
【0019】
【表1】

Figure 0003862873
【0020】
【発明の効果】
本発明によれば劣化した衣料の形態を回復させる繊維製品処理剤組成物を提供することができる。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a textile product treating agent composition.
[0002]
[Prior art and problems to be solved by the invention]
Currently, weak alkaline heavy detergents are usually used for washing clothes worn at home, and light detergents are used for washing clothes and the like. In addition, depending on taste, a softening agent that softens the clothing and a paste that hardens the clothing are used.
[0003]
However, repeated washing of the clothing will cause the collar and cuffs to shrink due to fiber damage, and the appearance and comfort will worsen due to lack of tension. Further, when such clothing is treated with a softening agent or a paste, there is a problem that the shape of the clothing is deformed or the original texture is impaired.
[0004]
Accordingly, an object of the present invention is to provide a treatment agent that restores the original shape and texture of clothing.
[0005]
[Means for Solving the Problems]
The present invention includes (A) a water-soluble processed starch having a weight average molecular weight of 5,000 to 500,000 and a derivative thereof and a water-soluble polymer compound selected from the group consisting of a water-soluble cellulose derivative having a weight average molecular weight of 10,000 to 500,000. %, (B) 0.5 to 5% by weight of a silicone compound and (C) a non-ionic surfactant of 0.1 to 5% by weight.
[0006]
DETAILED DESCRIPTION OF THE INVENTION
(A) The weight average molecular weight of the water-soluble processed starch of a component is 5000-500000, Preferably it is 10000-500000. As water-soluble processed starch, hydroxyethylated starch, hydroxypropylated starch, carboxymethylated starch, cationized starch having a quaternary ammonium group, or these can be reduced by an oxidizing agent (for example, H 2 O 2 , NaClO, etc.) or an enzyme. Viscosity is preferred. In this case, the degree of substitution indicating the ratio at which substituents such as hydroxyethyl group, carboxymethyl group and quaternary ammonium group are introduced to starch (the number of hydroxyl groups into which the substituents are introduced relative to the total number of hydroxyl groups of starch) The ratio is preferably 0.08 to 0.8, and more preferably 0.1 to 0.4, in terms of storage stability and texture.
[0007]
Examples of the water-soluble cellulose derivative of the component (A) include hydroxyalkyl celluloses such as hydroxymethyl cellulose, hydroxyethyl cellulose, and hydroxypropyl cellulose, alkyl celluloses such as methyl cellulose and ethyl cellulose, carboxymethyl cellulose, and cationized cellulose having a quaternary ammonium group. The weight average molecular weight is 10,000 to 500,000, preferably 50,000 to 200,000. These substitution degrees are 0.5 to 1.5, preferably 0.6 to 1.0.
[0008]
The weight average molecular weight of these water-soluble polymer compounds (A) is measured by gel permeation chromatography using polyethylene glycol as a standard substance.
[0009]
In the present invention, the water-soluble polymer compound refers to a compound in which 1 g of the water-soluble polymer compound is added to 100 g of water at 80 ° C. and the liquid becomes clear without becoming cloudy.
[0010]
Examples of the silicone compound as component (B) include dimethylpolysiloxane, methylphenylpolysiloxane, methylhydrogenpolysiloxane, amino-modified silicone, amide-modified silicone, epoxy-modified silicone, carboxy-modified silicone, and polyether-modified silicone. Particularly, dimethylpolysiloxane, amino-modified silicone, and polyether-modified silicone are preferable. The weight average molecular weight of the silicone compound is 1000 to 1000000, preferably 2000 to 100000. The weight average molecular weight of the silicone compound can be determined by gel permeation chromatography based on dimethylpolysiloxane having a known molecular weight. The silicone compound is preferably blended in the form of an aqueous emulsion in which particles are dispersed. The average particle diameter of the dispersed particles is 0.01 to 10 μm, particularly 0.01 to 0.5 μm, and further 0.05 to 0.00. 1 μm is good.
[0011]
As the nonionic surfactant of component (C), polyoxyalkylene alkyl or alkenyl ether, polyoxyalkylene alkyl phenyl ether, polyoxyalkylene sorbitan fatty acid ester, polyoxyalkylene glycol fatty acid ester, polyoxyethylene polyoxypropylene block Examples thereof include polymers. In particular, polyoxyethylene alkyl or alkenyl (C10-20) ether type nonionic surfactant is preferable. These preferably have an HLB of 12-18 by the Griffin method. As a particularly preferred component (C), the compounds of the following general formula (I) can be exemplified.
R- (OC 2 H 4) n -OH (I)
[Wherein, R is an alkyl group or alkenyl group having 12 to 20 carbon atoms, n is a number of 5 to 30, and R and n are adjusted so that HLB is in the range of 12 to 18. ]
Since the textile product treating agent composition of the present invention can provide a good garment shape recovery effect and texture-imparting effect, it contains 0.1 to 20% by weight, preferably 1 to 15% by weight of component (A). . In addition, the component (B) is 0.5 to 5% by weight, preferably 0.5 to 3% by weight, and the component (C) is 0.1 to 5% in terms of good storage stability and shape recovery effect. % By weight, preferably 0.3 to 3% by weight.
[0012]
The fiber product treating agent composition of the present invention may contain components used in ordinary softeners and pastes. Examples of such components include cationic surfactants, anionic surfactants, fragrances, dyes, antibacterial agents, solvents such as ethylene glycol and propylene glycol, inorganic salts such as sodium chloride, ammonium chloride, and calcium chloride. It is done.
[0013]
The textile product treating agent composition of the present invention contains the above components (A) to (C) and optional components, and the balance is usually water. The composition of the present invention is used after being diluted to an appropriate concentration. For example, the clothes are usually washed and processed at the rinsing stage by dissolving the composition of the present invention in water, or by using a container such as a tub to dissolve the composition of the present invention in water. Further, a method of immersing the clothes and putting them on can be considered. The fiber product may be treated by any method, but the concentration of the component (A) in the treatment bath is preferably 10 ppm to 1000 ppm, particularly 20 ppm to 500 ppm, and the bath ratio (treatment liquid for clothing) Is preferably 1/3 to 1/100, and more preferably 1/5 to 1/50.
[0014]
【Example】
<Preparation of textile product treating agent composition>
The composition shown in Table 1 was prepared. In addition, about each component, it is as follows.
[0015]
・ Cationized cellulose A-1
(Substitution degree 1.7-2.2, weight average molecular weight 150,000)
・ Cationized starch A-2
(Substitution degree 0.2-0.3, weight average molecular weight 100,000)
-Vinyl acetate-methacrylic acid copolymer water-dispersed emulsion A-3
(Effective content 40%, water-insoluble polymer)
・ Silicone B-1
[Toray Dow Corning Silicone Co., Ltd., SM8705, average particle size 0.03 to 0.04 μm, weight average molecular weight 80000]
・ Ditaroyldimethylammonium chloride B-2
・ Nonionic surfactant C-1
[Polyoxyethylene (average addition mole number 20) alkyl (carbon number 12) ether, HLB16.8]
・ Propylene glycol D-1
In addition, the solubility to the water of A-1 and A-2 was 1 g / 100g (80 degreeC) or more, and showed the clarity. Moreover, the solubility of A-3 in water was less than 0.01 g / 100 g (80 ° C.), and it was an emulsion.
[0016]
<Preparation of treated fiber products>
Five blue 100% cotton polo shirts were prepared, and four were washed 20 times with a commercially available heavy detergent using a National washing machine NA-F60E. The collars and cuffs of these four pieces of clothing are not stretched and have a fiber-like shape.
[0017]
<Processing method>
5 L of water was put into a 5 L tub, and 20 g of the composition shown in Table 1 was dissolved (A-1 or A-2 concentration 400 ppm, bath ratio = 1/30). One piece of the above-treated polo shirt was dipped for 10 minutes, then dehydrated in a washing machine and dried in the shade.
[0018]
<Evaluation criteria>
By the trained evaluator, the new polo shirt used above was compared with the form of the polo shirt subjected to the above-described treatment, and the evaluation was made according to the following criteria. The results are also shown in Table 1.
Recovered to the same form as the new one; +2
It does not recover until new, but has recovered to a satisfactory level; +1
Equivalent to untreated product; 0
[0019]
[Table 1]
Figure 0003862873
[0020]
【The invention's effect】
ADVANTAGE OF THE INVENTION According to this invention, the textiles processing agent composition which recovers the form of the deteriorated clothing can be provided.

Claims (1)

(A)重量平均分子量5000〜500000の水溶性加工澱粉及びその誘導体並びに重量平均分子量10000〜500000の水溶性セルロース誘導体からなる群から選ばれる水溶性高分子化合物0.1〜20重量%、(B)シリコーン化合物0.5〜5重量%及び(C)非イオン性界面活性剤0.1〜5重量%を含有する繊維製品処理剤組成物をすすぎ水に溶解させた、(A)の濃度が10ppm〜1000ppmである処理浴を用いて、すすぎの段階で繊維製品を処理する方法。 (A) 0.1 to 20% by weight of a water-soluble polymer compound selected from the group consisting of water-soluble processed starch having a weight average molecular weight of 5,000 to 500,000 and derivatives thereof and a water-soluble cellulose derivative having a weight average molecular weight of 10,000 to 500,000, (B (1) A textile product treating agent composition containing 0.5 to 5% by weight of a silicone compound and (C) 0.1 to 5% by weight of a nonionic surfactant was dissolved in rinse water, and the concentration of (A) was A method of treating a textile product at a rinsing stage using a treatment bath of 10 ppm to 1000 ppm.
JP29952398A 1998-10-21 1998-10-21 Textile treatment composition Expired - Fee Related JP3862873B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP29952398A JP3862873B2 (en) 1998-10-21 1998-10-21 Textile treatment composition

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP29952398A JP3862873B2 (en) 1998-10-21 1998-10-21 Textile treatment composition

Publications (2)

Publication Number Publication Date
JP2000129577A JP2000129577A (en) 2000-05-09
JP3862873B2 true JP3862873B2 (en) 2006-12-27

Family

ID=17873703

Family Applications (1)

Application Number Title Priority Date Filing Date
JP29952398A Expired - Fee Related JP3862873B2 (en) 1998-10-21 1998-10-21 Textile treatment composition

Country Status (1)

Country Link
JP (1) JP3862873B2 (en)

Families Citing this family (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004025017A1 (en) * 2002-09-13 2004-03-25 Lion Corporation Liquid fabric softener composition
TW200517556A (en) 2003-08-08 2005-06-01 Kao Corp Fabric product treating agent composition
JP4589622B2 (en) * 2003-12-25 2010-12-01 ライオン株式会社 Liquid softener composition
US7670388B2 (en) * 2005-10-14 2010-03-02 Kao Corporation Fiber-treating composition
JP4712664B2 (en) * 2005-10-14 2011-06-29 花王株式会社 Textile treatment composition and process for producing the same
JP4891837B2 (en) * 2006-10-02 2012-03-07 花王株式会社 Textile treatment composition
CN101675095B (en) 2007-04-11 2012-11-28 陶氏康宁公司 Silcone polyether block copolymers having organofunctional endblocking groups
JP2015526602A (en) * 2012-06-18 2015-09-10 ローディア オペレーションズ Fabric conditioning composition and uses thereof
CN104818618B (en) * 2015-04-30 2016-07-06 威莱(广州)日用品有限公司 A kind of wrinkle resistant ironing agent and preparation method thereof
PL3580318T3 (en) 2017-02-13 2023-10-02 Unilever Ip Holdings B.V. Method of delivering a laundry composition
BR112019016823B1 (en) 2017-02-13 2024-01-02 Unilever Ip Holdings B.V. AUXILIARY COMPOSITION FOR FABRIC WASHING, FABRIC WASHING METHOD AND USE OF THE AUXILIARY COMPOSITION FOR FABRIC WASHING
EP3580317B1 (en) 2017-02-13 2021-10-13 Unilever IP Holdings B.V. Laundry composition additive

Also Published As

Publication number Publication date
JP2000129577A (en) 2000-05-09

Similar Documents

Publication Publication Date Title
JP3862873B2 (en) Textile treatment composition
WO2019111949A1 (en) Fabric treatment composition
CA2276188A1 (en) Laundry detergent compositions with cellulosic polymers
US3920561A (en) Composition for imparting softness and soil release properties to fabrics
US4978462A (en) Compositions and process for the treatment of textiles comprising a resinous branched polyorganosiloxane and a polydiorganosiloxane in an aqueous dispersion
AU2019345048B2 (en) Home care compositions
DE69915329T2 (en) METHOD FOR WASHING SENSITIVE CLOTHING IN A WASHING MACHINE
US8618039B2 (en) Granular materials for finishing denim
JP4039750B2 (en) Liquid finish composition for textile products
WO2004025017A1 (en) Liquid fabric softener composition
JP3862874B2 (en) Textile treatment composition
JP2000129570A (en) Fiber product treating agent composition
JP4641814B2 (en) Textile treatment composition
JP2008297675A (en) Fiber product-treating agent composition
JP4275236B2 (en) Textile treatment agent
WO2005014921A1 (en) Fabric treating agent composition
JP4209073B2 (en) Liquid detergent composition
EP1723221B1 (en) Compositions useful as fabric softeners
JP4663106B2 (en) Cleaning composition
JP3208209B2 (en) Laundry aid composition
WO2019111937A1 (en) Washing agent composition for textile product
JP2001506706A (en) Rinse-added fabric conditioning compositions based on certain starches and methods of using the same
JP3612414B2 (en) Detergent composition for clothing
JP4408257B2 (en) Detergent composition
JP2683890B2 (en) Silk products

Legal Events

Date Code Title Description
A521 Written amendment

Free format text: JAPANESE INTERMEDIATE CODE: A523

Effective date: 20040818

A621 Written request for application examination

Free format text: JAPANESE INTERMEDIATE CODE: A621

Effective date: 20040818

A977 Report on retrieval

Free format text: JAPANESE INTERMEDIATE CODE: A971007

Effective date: 20060413

A131 Notification of reasons for refusal

Free format text: JAPANESE INTERMEDIATE CODE: A131

Effective date: 20060418

A521 Written amendment

Free format text: JAPANESE INTERMEDIATE CODE: A523

Effective date: 20060616

A131 Notification of reasons for refusal

Free format text: JAPANESE INTERMEDIATE CODE: A131

Effective date: 20060711

A521 Written amendment

Free format text: JAPANESE INTERMEDIATE CODE: A523

Effective date: 20060908

TRDD Decision of grant or rejection written
A01 Written decision to grant a patent or to grant a registration (utility model)

Free format text: JAPANESE INTERMEDIATE CODE: A01

Effective date: 20060926

A61 First payment of annual fees (during grant procedure)

Free format text: JAPANESE INTERMEDIATE CODE: A61

Effective date: 20060927

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

Free format text: PAYMENT UNTIL: 20101006

Year of fee payment: 4

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

Free format text: PAYMENT UNTIL: 20111006

Year of fee payment: 5

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

Free format text: PAYMENT UNTIL: 20121006

Year of fee payment: 6

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

Free format text: PAYMENT UNTIL: 20131006

Year of fee payment: 7

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

LAPS Cancellation because of no payment of annual fees