JPH0543894A - Bleaching agent and bleaching detergent composition - Google Patents

Bleaching agent and bleaching detergent composition

Info

Publication number
JPH0543894A
JPH0543894A JP20806791A JP20806791A JPH0543894A JP H0543894 A JPH0543894 A JP H0543894A JP 20806791 A JP20806791 A JP 20806791A JP 20806791 A JP20806791 A JP 20806791A JP H0543894 A JPH0543894 A JP H0543894A
Authority
JP
Japan
Prior art keywords
bleaching
acid
detergent composition
formula
binder
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
JP20806791A
Other languages
Japanese (ja)
Other versions
JP2925793B2 (en
Inventor
Shigemi Tsuchiya
滋美 土屋
Muneo Aoyanagi
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 JP20806791A priority Critical patent/JP2925793B2/en
Publication of JPH0543894A publication Critical patent/JPH0543894A/en
Application granted granted Critical
Publication of JP2925793B2 publication Critical patent/JP2925793B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Abstract

PURPOSE:To obtain a bleaching agent and a bleaching detergent composition having a stable bleaching effect, not decreasing in a bleaching effect even when stored for a long time and improved in powder properties by using granules prepared by granulating a mixture of phthalimidopercarboxylic acid and phthalimidocarboxylic acid in a specified ratio with a binder. CONSTITUTION:The title agent and composition are prepared from granules prepared by granulating a mixture of a compound (a) of formula I (wherein n is an integer of 1-15; and M is H, an alkali metal or an alkaline earth metal) with a compound (b) of formula II (wherein n and M are as defined above) in an (a) to (b) weight ratio of 95/5 to 50/50 with a binder of an m.p. of 30 deg.C or above.

Description

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

【0001】[0001]

【産業上の利用分野】本発明は漂白剤組成物、更に詳し
くは貯蔵時の安定性および粉末物性の改良された、フタ
ールイミドパーカルボン酸を含有する漂白剤及び漂白洗
浄剤組成物に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a bleaching composition, and more particularly to a bleaching agent and a bleaching detergent composition containing a phthalimide percarboxylic acid having improved stability during storage and powder properties.

【0002】[0002]

【従来の技術及びその課題】フタールイミドパーカルボ
ン酸は強い酸化力を有し、漂白剤基剤としての用途が期
待されている(特開平2−196771号、特開平2−1473
号、特開平2−76850号)。しかしながら、かかる化合
物を漂白剤組成物或いは漂白洗浄剤組成物の一成分とし
て配合するという検討はいまだ十分に行なわれていな
い。
BACKGROUND OF THE INVENTION Phthalimide percarboxylic acid has a strong oxidizing power and is expected to be used as a bleaching agent base (JP-A-2-196771 and JP-A-2-1473).
No. 2-76850). However, the study of incorporating such a compound as one component of a bleaching agent composition or a bleaching detergent composition has not yet been sufficiently conducted.

【0003】[0003]

【課題を解決するための手段】そこで、本発明者らは、
商品として市場に供給し得るフタールイミドパーカルボ
ン酸を含有する漂白剤及び漂白洗浄剤組成物について鋭
意研究した結果、フタールイミドパーカルボン酸とフタ
ールイミドカルボン酸を特定の重量比で混合した混合物
を結合剤で造粒して配合することにより、安定した漂白
効果を有し、しかも長期保存されても漂白効果の低下が
少なく、かつ粉末物性も劣化しない漂白剤及び漂白洗浄
剤組成物が得られることを見出し、本発明を完成した。
Therefore, the present inventors have
As a result of diligent research on a bleaching agent and a bleaching detergent composition containing a phthalimide percarboxylic acid which can be supplied to the market as a product, a phthalimide percarboxylic acid and a phthalimide carboxylic acid were mixed at a specific weight ratio. By blending the mixture by granulating the mixture with a binder, a bleaching agent and a bleaching detergent composition having a stable bleaching effect, less deterioration of the bleaching effect even after long-term storage, and powder properties are not deteriorated The inventors have found that they can be obtained and completed the present invention.

【0004】即ち、本発明は、(a) 下記の一般式(I)That is, the present invention provides (a) the following general formula (I)

【0005】[0005]

【化3】 [Chemical 3]

【0006】〔式中、n は1〜15の整数、M は H又はア
ルカリ金属原子又はアルカリ土類金属原子を表す。〕で
表される化合物及び(b) 下記の一般式(II)
[In the formula, n represents an integer of 1 to 15, M represents H or an alkali metal atom or an alkaline earth metal atom. ] And a compound represented by the following general formula (II)

【0007】[0007]

【化4】 [Chemical 4]

【0008】〔式中、n は1〜15の整数、M は H又は
アルカリ金属原子又はアルカリ土類金属原子を表す。〕
で表される化合物を、(a) /(b) 重量比で95/5〜50/
50の範囲で含有する混合物を、融点が30℃以上の結合剤
で造粒した造粒物を配合してなる漂白剤及び漂白洗浄剤
組成物を提供するものである。
[In the formula, n represents an integer of 1 to 15, M represents H or an alkali metal atom or an alkaline earth metal atom. ]
The compound represented by the formula (a) / (b) in a weight ratio of 95/5 to 50 /
A bleaching agent and a bleaching detergent composition are prepared by blending a granulated product obtained by granulating a mixture containing 50 parts by weight with a binder having a melting point of 30 ° C. or higher.

【0009】本発明で使用される(a) 成分のフタールイ
ミドパーカルボン酸は、下記一般式(I)
The (a) component phthalimido percarboxylic acid used in the present invention has the following general formula (I):

【0010】[0010]

【化5】 [Chemical 5]

【0011】〔式中、n は1〜15の整数、M は H又はア
ルカリ金属原子又はアルカリ土類金属原子を表す。〕で
表わされる化合物であり、中でも一般式(I) 中のn が
5、M がH である化合物が安定性、生分解性が特に良好
であり好ましい。
[In the formula, n represents an integer of 1 to 15, M represents H or an alkali metal atom or an alkaline earth metal atom. ] Among them, the compound represented by the formula (I) in which n is 5 and M is H is particularly preferable because of its excellent stability and biodegradability.

【0012】また、一般式(II)のフタールイミドカルボ
ン酸は、使用する一般式(I) のフタールイミドパーカル
ボン酸と同じn 数を有する場合に特に安定化効果が良好
である。
Further, the phthalimidocarboxylic acid of the general formula (II) has a particularly good stabilizing effect when it has the same n number as the phthalimidopercarboxylic acid of the general formula (I) used.

【0013】フタールイミドパーカルボン酸(a) とフタ
ールイミドカルボン酸(b) は造粒物中に(a) /(b) =95
/5〜50/50、好ましくは90/10〜60/30の重量比で配
合される。また、造粒物中の (a)+(b) 総量は15〜90重
量%である。フタールイミドカルボン酸の比率が少ない
と十分な安定化効果が得られず、また多く配合しても安
定化効果は飽和する。
The phthalimidopercarboxylic acid (a) and the phthalimidocarboxylic acid (b) are (a) / (b) = 95 in the granulated product.
It is blended in a weight ratio of / 5 to 50/50, preferably 90/10 to 60/30. The total amount of (a) + (b) in the granulated product is 15 to 90% by weight. When the ratio of the phthalimidocarboxylic acid is small, a sufficient stabilizing effect cannot be obtained, and even when the ratio is large, the stabilizing effect is saturated.

【0014】フタールイミドパーカルボン酸(a) とフタ
ールイミドカルボン酸(b) は、造粒物の保存安定性の面
から、融点が30℃以上、好ましくは45℃以上、特に好ま
しくは50〜90℃の結合剤、例えばポリエチレングリコー
ル、ポリオキシエチレンアルキルエーテル及び高級脂肪
酸から選ばれる1種又は2種以上の化合物を結合剤とし
て用い、造粒されたものを使用する。これらの結合剤は
造粒物中に好ましくは2〜30重量%、特に好ましくは5
〜20重量%使用するのが望ましい。
From the viewpoint of storage stability of the granulated product, the phthalimido percarboxylic acid (a) and the phthalimido carboxylic acid (b) have a melting point of 30 ° C. or higher, preferably 45 ° C. or higher, and particularly preferably 50. A granulated product is used by using a binder at 90 ° C, for example, one or more compounds selected from polyethylene glycol, polyoxyethylene alkyl ethers and higher fatty acids as a binder. These binders are preferably contained in the granulated product in an amount of 2 to 30% by weight, particularly preferably 5%.
It is desirable to use ~ 20% by weight.

【0015】造粒物の製造方法は特に限定されるもので
はないが、例えば結合剤の融点以上の温度でフタールイ
ミドパーカルボン酸(a) 及びフタールイミドカルボン酸
(b)粉末と混合攪拌する方法、結合剤高濃度水溶液又は
溶融物を添加又は噴霧しながら混合攪拌する方法などが
ある。必要によっては、フタールイミドパーカルボン酸
の衝撃感度を軽減するため及び貯蔵安定性を改善するた
めに、フタールイミドパーカルボン酸に不活性の希釈剤
0.5〜70重量%の共存下に造粒される。希釈剤として
は、硫酸塩、重硫酸塩、炭酸塩、重炭酸塩、硝酸塩、オ
ルトリン酸塩、ピロリン酸塩、ポリリン酸塩、セルロー
ス系物質、デンプン系物質等が挙げられる。希釈剤とし
て特に好ましいものは結晶水を取り得る平均水分含量5
%以下の実質的に無水の物質であり、無水炭酸ナトリウ
ム、無水トリポリリン酸ナトリウム、無水ピロリン酸ナ
トリウム、無水リン酸三ナトリウム、無水メタケイ酸ナ
トリウム、無水ニトリロトリ酢酸ナトリウム、無水硫酸
マグネシウム、無水塩化カルシウム、無水硫酸ナトリウ
ム及び無水クエン酸ナトリウム等が例示される。中でも
無水硫酸マグネシウム、無水塩化カルシウム、無水硫酸
ナトリウム及び無水クエン酸ナトリウムが特に好まし
い。
The method for producing the granulated product is not particularly limited, but for example, phthalimidopercarboxylic acid (a) and phthalimidocarboxylic acid can be used at a temperature above the melting point of the binder.
(b) A method of mixing and stirring with powder, a method of mixing and stirring while adding or spraying a binder high-concentration aqueous solution or a melt. If necessary, in order to reduce the impact sensitivity of the phthalimido percarboxylic acid and to improve the storage stability, a diluent inert to the phthal imide percarboxylic acid is used.
Granulated in the coexistence of 0.5 to 70% by weight. Examples of the diluent include sulfates, bisulfates, carbonates, bicarbonates, nitrates, orthophosphates, pyrophosphates, polyphosphates, cellulosics, and starches. Particularly preferred as the diluent is an average water content of 5 which can take water of crystallization.
% Or less of substantially anhydrous substance, anhydrous sodium carbonate, anhydrous sodium tripolyphosphate, anhydrous sodium pyrophosphate, anhydrous trisodium phosphate, anhydrous sodium metasilicate, anhydrous sodium nitrilotriacetate, anhydrous magnesium sulfate, anhydrous calcium chloride, Examples include anhydrous sodium sulfate and anhydrous sodium citrate. Among them, anhydrous magnesium sulfate, anhydrous calcium chloride, anhydrous sodium sulfate and anhydrous sodium citrate are particularly preferable.

【0016】このようにして得られた平均粒径 300〜20
00μ、好ましくは 300〜1000μの造粒物が本発明の漂白
剤及び漂白洗浄剤組成物に使用される。造粒物はフター
ルイミドパーカルボン酸として漂白剤及び漂白洗浄剤組
成物中に 0.5〜80重量%、好ましくは2〜60重量%配合
される。
The average particle size thus obtained is 300 to 20
Granules of 00μ, preferably 300-1000μ, are used in the bleach and bleach detergent compositions of the present invention. The granulated product is added as a phthalimido percarboxylic acid in the bleaching agent and the bleaching detergent composition in an amount of 0.5 to 80% by weight, preferably 2 to 60% by weight.

【0017】本発明の漂白剤及び漂白洗浄剤組成物中に
は、上記(a),(b)成分の他に、洗浄剤常用成分、例えば
次のような成分を配合できる。アルキルベンゼンスルホ
ン酸塩、アルキルエーテル硫酸塩、アルキル硫酸塩、オ
レフィンスルホン酸塩、アルカンスルホン酸塩、高級脂
肪酸塩、α−スルホ脂肪酸塩又はエステル等のアニオン
界面活性剤、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、ポリオキシエチレンフェニルエーテル、
高級脂肪酸アルカノールアミド又はそのアルキレンオキ
サイド付加物、アルキルグリコシド、アルキルアミンオ
キサイド等のノニオン界面活性剤、ベタイン型両性界面
活性剤、スルホン酸型両性界面活性剤、カチオン性界面
活性剤等の界面活性剤;ケイ酸塩、炭酸塩、セスキ炭酸
塩(Na, K, Mg塩等) 等のアルカリ剤及び硫酸塩等の増量
剤;オルトリン酸塩、ピロリン酸塩、トリポリリン酸
塩、クエン酸塩、イソクエン酸塩、エチレンジアミン四
酢酸塩、ニトリロ三酢酸塩、ポリアクリル酸塩、ポリア
セタールカルボン酸塩、ゼオライト等の2価金属イオン
捕捉剤;ポリビニルアルコール、ポリビニルピロリド
ン、カルボキシメチルセルロース、ポリエチレングリコ
ール等の再汚染防止剤;プロテアーゼ、エスペラーゼ、
リパーゼ、セルラーゼなどの酵素;過炭酸ソーダ、過硼
酸ソーダ等のその他の漂白剤、2−ヒドロキシエチルイ
ミノ二酢酸塩等の脱褪色防止剤;その他ケーキング防止
剤、漂白活性化剤、酸化防止剤、蛍光染料、青味付剤、
光活性化漂白剤、香料等。
In the bleaching agent and the bleaching detergent composition of the present invention, in addition to the above-mentioned components (a) and (b), common detergent ingredients, for example, the following ingredients can be added. Alkylbenzene sulfonate, alkyl ether sulfate, alkyl sulfate, olefin sulfonate, alkane sulfonate, higher fatty acid salt, anionic surfactant such as α-sulfo fatty acid salt or ester, polyoxyalkylene alkyl or alkenyl ether, Polyoxyethylene phenyl ether,
Nonionic surfactants such as higher fatty acid alkanolamides or alkylene oxide adducts thereof, alkyl glycosides, alkylamine oxides, betaine type amphoteric surfactants, sulfonic acid type amphoteric surfactants, cationic surfactants and other surfactants; Alkaline agents such as silicates, carbonates, sesquicarbonates (Na, K, Mg salts, etc.) and extenders such as sulfates; orthophosphates, pyrophosphates, tripolyphosphates, citrates, isocitrates , Ethylenediaminetetraacetate, nitrilotriacetate, polyacrylate, polyacetalcarboxylate, zeolite and other divalent metal ion scavengers; polyvinyl alcohol, polyvinylpyrrolidone, carboxymethylcellulose, polyethylene glycol, etc. recontamination inhibitors; proteases , Esperase,
Enzymes such as lipase and cellulase; other bleaching agents such as sodium percarbonate and sodium perborate; anti-fading agents such as 2-hydroxyethyliminodiacetic acid salt; other anti-caking agents, bleach activators, antioxidants, Fluorescent dye, bluing agent,
Light activated bleach, fragrance, etc.

【0018】[0018]

【実施例】以下に実施例を示し本発明を詳細に説明する
が、本発明はこれらの実施例に制約されるものではな
い。
The present invention will be described in detail below with reference to examples, but the present invention is not limited to these examples.

【0019】実施例1 表1の配合組成からなる造粒物(粒径 350〜710 μ)を
調製した。即ちフタールイミドパーカルボン酸〔一般式
(I) 中のn =5〕とフタールイミドカルボン酸〔一般式
(II)中のn =5〕、比較品の場合は脂肪酸を混合し、ポ
リエチレングリコール(重量平均分子量=6000, 融点56
〜63℃)を添加しながら混合造粒した。得られた造粒物
を空気抜き程度の小さなすきまを開けた 300ccのポリボ
トルに150 g入れ、40℃で一ケ月間保存した後、以下の
方法で保存安定性の評価を有効酸素の残存率と粉末物性
により行った。その結果を表1に示す。
Example 1 Granules (particle size 350 to 710 μm) having the blending composition shown in Table 1 were prepared. That is, phthalimido percarboxylic acid [general formula
N = 5] in (I) and phthalimidocarboxylic acid [general formula
N = 5 in (II)], in the case of the comparative product, a fatty acid was mixed, and polyethylene glycol (weight average molecular weight = 6000, melting point 56
(About 63 ° C.) and mixed granulation. Put 150 g of the obtained granules in a 300 cc plastic bottle with a small gap for air bleeding, store at 40 ° C for 1 month, and then evaluate the storage stability by the following method. The physical properties were used. The results are shown in Table 1.

【0020】[0020]

【数1】 [Equation 1]

【0021】(2) 粉末物性 ○:固まりがない ×:固まりがある(2) Physical properties of powder: ◯: no lump x: lump

【0022】[0022]

【表1】 [Table 1]

【0023】注) *1 PEG;ポリエチレングリコール(重量平均分子量=60
00, 融点56〜63℃) 実施例2 実施例1で調製した表1中の本発明品1及び比較品1
に、更に表2に示す成分を添加して造粒物を調製した。
尚、表中のE 510はポリオキシエチレンアルキルエーテ
ル(C12/C13/C14=21.9/52.0/26.1)エチレンオキサイ
ド10モル付加物であり、E 911 はポリオキシエチレンノ
ニルフェニルエーテルエチレンオキサイド11モル付加物
であり、LAS はドデシルベンゼンスルホネートであり、
これらは予め炭酸ナトリウム及び炭酸水素ナトリウムと
混合し、含浸させて配合した。得られた造粒物を用いて
実施例1と同様の試験を行なった。その結果を表2に示
す。
Note) * 1 PEG; polyethylene glycol (weight average molecular weight = 60
00, melting point 56-63 ° C.) Example 2 Inventive product 1 and comparative product 1 in Table 1 prepared in Example 1
Further, the ingredients shown in Table 2 were added to prepare a granulated product.
In the table, E 510 is a polyoxyethylene alkyl ether (C 12 / C 13 / C 14 = 21.9 / 52.0 / 26.1) ethylene oxide 10 mol adduct, and E 911 is polyoxyethylene nonylphenyl ether ethylene oxide 11 Is a molar adduct, LAS is dodecylbenzene sulfonate,
These were mixed in advance with sodium carbonate and sodium hydrogen carbonate, impregnated and blended. The same test as in Example 1 was performed using the obtained granulated product. The results are shown in Table 2.

【0024】[0024]

【表2】 [Table 2]

───────────────────────────────────────────────────── 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 C11D 7:38) ─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 5 Identification code Office reference number FI technical display location C11D 7:38)

Claims (1)

【特許請求の範囲】[Claims] 【請求項1】 (a) 下記の一般式(I) 【化1】 〔式中、n は1〜15の整数、M は H又はアルカリ金属原
子又はアルカリ土類金属原子を表す。〕で表される化合
物及び(b) 下記の一般式(II) 【化2】 〔式中、n は1〜15の整数、M は H又はアルカリ金属原
子又はアルカリ土類金属原子を表す。〕で表される化合
物を、(a) /(b) 重量比で95/5〜50/50の範囲で含有
する混合物を、融点が30℃以上の結合剤で造粒した造粒
物を配合してなる漂白剤及び漂白洗浄剤組成物。
1. (a) The following general formula (I): [In the formula, n represents an integer of 1 to 15, M represents H or an alkali metal atom or an alkaline earth metal atom. ] And a compound represented by the following general formula (II): [In the formula, n represents an integer of 1 to 15, M represents H or an alkali metal atom or an alkaline earth metal atom. ] A compound containing the compound represented by (a) / (b) in a weight ratio range of 95/5 to 50/50, and a granulated product obtained by granulating with a binder having a melting point of 30 ° C or higher. A bleaching agent and a bleaching detergent composition.
JP20806791A 1991-08-20 1991-08-20 Bleach and bleach detergent composition Expired - Fee Related JP2925793B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP20806791A JP2925793B2 (en) 1991-08-20 1991-08-20 Bleach and bleach detergent composition

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP20806791A JP2925793B2 (en) 1991-08-20 1991-08-20 Bleach and bleach detergent composition

Publications (2)

Publication Number Publication Date
JPH0543894A true JPH0543894A (en) 1993-02-23
JP2925793B2 JP2925793B2 (en) 1999-07-28

Family

ID=16550100

Family Applications (1)

Application Number Title Priority Date Filing Date
JP20806791A Expired - Fee Related JP2925793B2 (en) 1991-08-20 1991-08-20 Bleach and bleach detergent composition

Country Status (1)

Country Link
JP (1) JP2925793B2 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH11209796A (en) * 1998-01-29 1999-08-03 Kao Corp Bleaching agent composition for hard article
WO2012076345A1 (en) * 2010-12-06 2012-06-14 L'oreal Cosmetic composition comprising an imidoperoxycarboxylic acid, an imidocarboxylic acid and copolymer of 2-acrylamido-2-methylpropanesulphonic acid

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH11209796A (en) * 1998-01-29 1999-08-03 Kao Corp Bleaching agent composition for hard article
WO2012076345A1 (en) * 2010-12-06 2012-06-14 L'oreal Cosmetic composition comprising an imidoperoxycarboxylic acid, an imidocarboxylic acid and copolymer of 2-acrylamido-2-methylpropanesulphonic acid

Also Published As

Publication number Publication date
JP2925793B2 (en) 1999-07-28

Similar Documents

Publication Publication Date Title
EP1945850B1 (en) Non-aqueous liquid oxygen bleach composition
JP2801754B2 (en) Bleach composition
JP2925793B2 (en) Bleach and bleach detergent composition
JP2648074B2 (en) Tablet type detergent composition
JP2869310B2 (en) Stable sodium percarbonate, method for producing the same, and bleaching detergent composition containing stable sodium percarbonate
JP5779419B2 (en) Powder cleaning composition
JP2009126932A (en) Granular bleaching activator
JPS5851999B2 (en) bleach composition
EP0365170A1 (en) Detergent composition
JP2756026B2 (en) Bleach composition
JP2758547B2 (en) Bleach detergent composition
JP3246843B2 (en) Nonionic powder detergent composition
JP2000178594A (en) Bleaching detergent composition
JPH03115496A (en) Bleaching agent and bleaching detergent composition
JP2018030907A (en) Powder bleaching agent
JP4534193B2 (en) Powder detergent composition
JP2831920B2 (en) Bleach detergent composition
JPH0543899A (en) Nonionic powdery bleaching detergent composition
JP3628824B2 (en) Bleach activator granules
JP2978275B2 (en) Bleach composition
JP2771943B2 (en) Bleach detergent composition
JP3164794B2 (en) Cleaning composition
JPH09111290A (en) Granular bleaching agent composition
JP2771942B2 (en) Bleach detergent composition
JPH0662995B2 (en) Bleaching detergent composition

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

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: 10

Free format text: PAYMENT UNTIL: 20090507

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

Free format text: PAYMENT UNTIL: 20090507

Year of fee payment: 10

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

Year of fee payment: 11

Free format text: PAYMENT UNTIL: 20100507

LAPS Cancellation because of no payment of annual fees