JP2010235509A - Microorganism controlling agent and microorganism controlling method - Google Patents

Microorganism controlling agent and microorganism controlling method Download PDF

Info

Publication number
JP2010235509A
JP2010235509A JP2009085033A JP2009085033A JP2010235509A JP 2010235509 A JP2010235509 A JP 2010235509A JP 2009085033 A JP2009085033 A JP 2009085033A JP 2009085033 A JP2009085033 A JP 2009085033A JP 2010235509 A JP2010235509 A JP 2010235509A
Authority
JP
Japan
Prior art keywords
dimethyliminio
poly
methyl
microorganism controlling
ethylene
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
JP2009085033A
Other languages
Japanese (ja)
Other versions
JP5356884B2 (en
Inventor
Hiroaki Inoue
浩章 井上
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.)
Aquas Corp
Original Assignee
Aquas 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 Aquas Corp filed Critical Aquas Corp
Priority to JP2009085033A priority Critical patent/JP5356884B2/en
Publication of JP2010235509A publication Critical patent/JP2010235509A/en
Application granted granted Critical
Publication of JP5356884B2 publication Critical patent/JP5356884B2/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

<P>PROBLEM TO BE SOLVED: To provide a microorganism controlling agent having a high microorganism controlling capability even in a low concentration while maintaining its effect, and a microorganism controlling method. <P>SOLUTION: The microorganism controlling agent includes, as the active components, poly[oxyethylene(dimethyliminio)ethylene(dimethyliminio)ethylene dichloride] and/or poly(2-hydroxypropyldimethylammonium chloride) and 2-methyl-4-isothiazoline-3-one. <P>COPYRIGHT: (C)2011,JPO&INPIT

Description

本発明は、開放循環冷却水系などの水系水に対する微生物防除剤、及び、微生物防除方法に関する。   The present invention relates to a microbial control agent and a microbial control method for aqueous water such as an open circulation cooling water system.

開放循環冷却水系における微生物防除剤、特に細菌防除剤として、イソチアゾロン系化合物、特に5−クロロ−2−メチル−4−イソチアゾリン−3−オンは、抗菌スペクトルが広く、水溶性で取扱いが容易、かつ、低毒性なことから広く使われてきた(特公昭58−4682号公報(特許文献1))。   As a microorganism control agent in an open circulating cooling water system, particularly as a bacterial control agent, isothiazolone compounds, particularly 5-chloro-2-methyl-4-isothiazolin-3-one has a wide antibacterial spectrum, is water-soluble and easy to handle, and It has been widely used because of its low toxicity (Japanese Patent Publication No. 58-4682 (Patent Document 1)).

しかし、5−クロロ−2−メチル−4−イソチアゾリン−3−オンは不安定で分解速度が速いために効果の持続性には難点があり、この点を改善する長期間安定なスライムコントロ−ル剤として、2−メチル−4−イソチアゾリン−3−オンが提案されている(特開2002−193712公報(特許文献2))。   However, since 5-chloro-2-methyl-4-isothiazolin-3-one is unstable and has a high decomposition rate, there is a difficulty in sustaining the effect, and a long-term stable slime control that improves this point. 2-Methyl-4-isothiazolin-3-one has been proposed as an agent (Japanese Patent Laid-Open No. 2002-193712 (Patent Document 2)).

この技術によれば、従来の問題点である効果の持続性には格段の改善は見られるものの、2−メチル−4−イソチアゾリン−3−オンは、5−クロロ−2−メチル−4−イソチアゾリン−3−オンと比較して殺菌力自体が弱いために、効果を発揮させるために多量の薬剤の添加が必要となるという問題が生じる。   According to this technique, although the improvement in the sustainability of the effect, which is a problem in the past, is markedly improved, 2-methyl-4-isothiazolin-3-one is a 5-chloro-2-methyl-4-isothiazoline. Since the sterilizing power itself is weaker than that of -3-one, there arises a problem that a large amount of a drug needs to be added to exert the effect.

特公昭58−4682号公報Japanese Patent Publication No.58-4682 特開2002−193712公報JP 2002-193712 A

本発明は、効果の持続性を維持しながら、低濃度での添加であっても、高い微生物防除性能を有する微生物防除剤、及び、微生物防除方法を提供することを目的とするものである。   An object of the present invention is to provide a microbial control agent and a microbial control method having high microbial control performance even when added at a low concentration while maintaining the sustainability of the effect.

本発明は、このような問題点を解決する、すなわち、特定のカチオンポリマ−と2−メチル−4−イソチアゾリン−3−オンとを併用することにより、効果の持続性を維持しながら低濃度の添加であっても高い殺菌効果を示すことを見出し、本発明に至った。   The present invention solves such problems, that is, by using a specific cationic polymer in combination with 2-methyl-4-isothiazolin-3-one, a low concentration can be maintained while maintaining the durability of the effect. Even if it was added, it was found that a high bactericidal effect was exhibited, and the present invention was achieved.

すなわち、本発明の微生物防除剤は、請求項1に記載の通り、ポリ[オキシエチレン(ジメチルイミニオ)エチレン(ジメチルイミニオ)エチレンジクロライド]、及び/または、ポリ(2−ヒドロキシプロピルジメチルアンモニウムクロライド)と、2−メチル−4−イソチアゾリン−3−オンと、を有効成分として含有することを特徴とする微生物防除剤である。   That is, the microorganism control agent of the present invention is poly [oxyethylene (dimethyliminio) ethylene (dimethyliminio) ethylene dichloride] and / or poly (2-hydroxypropyldimethylammonium chloride) as described in claim 1. ) And 2-methyl-4-isothiazolin-3-one as an active ingredient.

また、本発明の微生物防除方法は、請求項2に記載の通り、ポリ[オキシエチレン(ジメチルイミニオ)エチレン(ジメチルイミニオ)エチレンジクロライド]、及び/または、ポリ(2−ヒドロキシプロピルジメチルアンモニウムクロライド)と、2−メチル−4−イソチアゾリン−3−オンと、を有効成分として水系水に添加することを特徴とする微生物防除方法である。   In addition, the method for controlling microorganisms of the present invention comprises poly [oxyethylene (dimethyliminio) ethylene (dimethyliminio) ethylene dichloride] and / or poly (2-hydroxypropyldimethylammonium chloride) according to claim 2. ) And 2-methyl-4-isothiazolin-3-one as an active ingredient is added to aqueous water.

本発明は、ポリ[オキシエチレン(ジメチルイミニオ)エチレン(ジメチルイミニオ)エチレンジクロライド]、及び/または、ポリ(2−ヒドロキシプロピルジメチルアンモニウムクロライド)を、2−メチル−4−イソチアゾリン−3−オンと併用することにより、優れた殺菌効果を持続させることができ、これらを組み合わせて微生物防除対象水系水へ添加することにより、効果の持続性を維持しながら低濃度の添加であっても高い殺菌効果を得ることができる。   The present invention relates to poly [oxyethylene (dimethyliminio) ethylene (dimethyliminio) ethylene dichloride] and / or poly (2-hydroxypropyldimethylammonium chloride) as 2-methyl-4-isothiazolin-3-one. Can be used to maintain excellent sterilization effects, and by combining them and adding them to the microbial control target water system, high sterilization can be achieved even at low concentrations while maintaining the sustainability of the effects. An effect can be obtained.

本発明において、ポリ[オキシエチレン(ジメチルイミニオ)エチレン(ジメチルイミニオ)エチレンジクロライド]、及び/または、ポリ(2−ヒドロキシプロピルジメチルアンモニウムクロライド)と、2−メチル−4−イソチアゾリン−3−オンと、は、重量比で1:100〜100:1となるように用いることが高い効果が得られるので好ましい。さらに好ましい範囲は1:10〜10:1である。これら薬剤は水に溶解して1剤としても安定している。   In the present invention, poly [oxyethylene (dimethyliminio) ethylene (dimethyliminio) ethylene dichloride] and / or poly (2-hydroxypropyldimethylammonium chloride) and 2-methyl-4-isothiazolin-3-one Are preferably used in a weight ratio of 1: 100 to 100: 1 because a high effect can be obtained. A more preferred range is 1:10 to 10: 1. These drugs dissolve in water and are stable as a single agent.

ポリ[オキシエチレン(ジメチルイミニオ)エチレン(ジメチルイミニオ)エチレンジクロライド]、及び/または、ポリ(2−ヒドロキシプロピルジメチルアンモニウムクロライド)と、2−メチル−4−イソチアゾリン−3−オンと、は、微生物防除目的の水系水に対して、有効成分の合計添加濃度として2mg/L以上1000mg/L以下となるように添加することが好ましい。添加濃度が2mg/L未満であると充分な効果が得られないときがあり、また、1000mg/Lを超えて添加しても、添加量の増加に見合う除菌効果の増加は得られにくい。最適な添加範囲は10mg/L以上100mg/L以下である。   Poly [oxyethylene (dimethyliminio) ethylene (dimethyliminio) ethylene dichloride] and / or poly (2-hydroxypropyldimethylammonium chloride) and 2-methyl-4-isothiazolin-3-one are: It is preferable to add to the aqueous water for the purpose of controlling the microorganism so that the total concentration of the active ingredients is 2 mg / L or more and 1000 mg / L or less. If the addition concentration is less than 2 mg / L, a sufficient effect may not be obtained, and even if the addition concentration exceeds 1000 mg / L, an increase in the sterilization effect commensurate with the increase in the addition amount is difficult to obtain. The optimal addition range is 10 mg / L or more and 100 mg / L or less.

本発明の微生物防除剤では、本発明の効果が妨げられない範囲で、さらにその特性を改良するなどの目的で、例えばアクリル酸系、マレイン酸系、メタクリル酸系、スルホン酸系、イタコン酸系、または、イソブチレン系の各重合体やこれらの共重合体、燐酸系重合体、ホスホン酸、ホスフィン酸、あるいはこれらの水溶性塩、などのスケール防止剤、例えば5-クロロ−2−メチル−4−イソチアゾリン−3−オン、1,2−ベンズイソチアゾリン−3−オン等の2−メチル−4−イソチアゾリン−3−オン以外のイソチアゾリン系化合物、グルタルアルデヒド、フタルアルデヒド等のアルデヒド系化合物、過酸化水素、ヒドラジン、塩素系殺菌剤(次亜塩素酸ナトリウム等)、臭素系殺菌剤およびヨウ素系殺菌剤、さらにピリチオン系化合物、ジチオール系化合物、メチレンビスチオシアネートなどのチオシアネート系化合物、四級アンモニウム塩系化合物、四級ホスホニウム塩系化合物、ピリジニウム塩系化合物、ポリ[オキシエチレン(ジメチルイミニオ)エチレン(ジメチルイミニオ)エチレンジクロライド]及びポリ(2−ヒドロキシプロピルジメチルアンモニウムクロライド)以外のヨーネンポリマー等のカチオン系化合物、などのスライム防止剤、例えばベンゾトリアゾール、トリルトリアゾール等のアゾール類、例えばエチレンジアミン、ジエチレントリアミン等のアミン系化合物、例えばニトリロ三酢酸、エチレンジアミン四酢酸、ジエチレントリアミン五酢酸等のアミノカルボン酸系化合物、例えばグルコン酸、クエン酸、シュウ酸、ギ酸、酒石酸、フィチン酸、琥珀酸、乳酸等の有機カルボン酸など、各種の水処理剤を添加することができ、その場合も本発明に含まれる。   In the microorganism control agent of the present invention, for the purpose of further improving the characteristics within the range where the effects of the present invention are not hindered, for example, acrylic acid-based, maleic acid-based, methacrylic acid-based, sulfonic acid-based, itaconic acid-based Or scale inhibitors such as isobutylene polymers, copolymers thereof, phosphoric acid polymers, phosphonic acid, phosphinic acid, or water-soluble salts thereof, such as 5-chloro-2-methyl-4 -Isothiazoline compounds other than 2-methyl-4-isothiazolin-3-one such as isothiazoline-3-one and 1,2-benzisothiazolin-3-one, aldehyde compounds such as glutaraldehyde and phthalaldehyde, hydrogen peroxide , Hydrazine, chlorine-based disinfectants (such as sodium hypochlorite), bromine-based and iodine-based disinfectants, and pyrithione compounds Products, dithiol compounds, thiocyanate compounds such as methylenebisthiocyanate, quaternary ammonium salt compounds, quaternary phosphonium salt compounds, pyridinium salt compounds, poly [oxyethylene (dimethyliminio) ethylene (dimethyliminio) ethylene Anti-slime agents such as cationic compounds such as ionene polymers other than dichloride and poly (2-hydroxypropyldimethylammonium chloride), azoles such as benzotriazole and tolyltriazole, and amine compounds such as ethylenediamine and diethylenetriamine Aminocarboxylic acid compounds such as nitrilotriacetic acid, ethylenediaminetetraacetic acid, diethylenetriaminepentaacetic acid, such as gluconic acid, citric acid, oxalic acid, formic acid, tartaric acid, phytin , Succinic acid, and organic carboxylic acids such as lactic acid, can be added to various water treatment agent, in which case is also included in the present invention.

<実施例1>
茨城県内にある工場の冷却水系より採取した冷却水を試験水として使用した。
<Example 1>
Cooling water collected from the cooling water system of a factory in Ibaraki Prefecture was used as test water.

上記試験水を30mLずつ50mLの振盪フラスコに採り、表1に示した薬品(略号も併せて示す)を表2に示す濃度(表中単位はmg/L。表中、各空欄は「添加なし」を表す)で添加し、その後30℃、60rpmで振盪培養した。培養開始72時間後に試験水中の一般細菌数をJIS K0101 63.2に従って測定した。   Take 30 mL of the test water in a 50 mL shake flask and concentrate the chemicals shown in Table 1 (also abbreviations are shown) in Table 2 (units in mg / L in the table. ”, And then cultured with shaking at 30 ° C. and 60 rpm. After 72 hours from the start of culture, the number of general bacteria in the test water was measured according to JIS K0101 63.2.

測定結果を表2に併せて示す(表中”<10”は10個/mL未満であることを示す)。なお、試験開始時の試験水の一般細菌数は3500個/mLであった。   The measurement results are also shown in Table 2 (“<10” in the table indicates less than 10 / mL). The general bacterial count of test water at the start of the test was 3500 cells / mL.

Figure 2010235509
Figure 2010235509

Figure 2010235509
Figure 2010235509

表2により、A〜Eの各種カチオンポリマーのうち、本発明にかかるカチオンポリマーであるAまたはBと2−メチル−4−イソチアゾリン−3−オンとの組み合わせからなる微生物防除剤が、他の組み合わせでの使用または単剤での使用と比較して、極めて高い相乗的な微生物防除性能を有していることが判る。   According to Table 2, among various cationic polymers of A to E, a microorganism control agent comprising a combination of A or B which is a cationic polymer according to the present invention and 2-methyl-4-isothiazolin-3-one is another combination. It can be seen that it has an extremely high synergistic microbial control performance as compared with the use in a single agent or a single agent.

<実施例2>
東京都内にあるビルの空調用の冷却水系より採取した冷却水を試験水として使用した。
<Example 2>
Cooling water collected from the cooling water system for air conditioning in buildings in Tokyo was used as test water.

上記試験水を30mLずつ50mLの振盪フラスコに採り、表3に示した薬品(略号も併せて示す)を表4に示す濃度(表中単位はmg/L。表中、各空欄は「添加なし」を表す)で添加し、その後30℃、60rpmで振盪培養した。培養開始24、72及び168時間後にそれぞれ試験水中の一般細菌数をJIS K0101 63.2に従って測定した。   Each 30 mL of the above test water was placed in a 50 mL shake flask, and the concentrations shown in Table 3 for the chemicals shown in Table 3 (abbreviations are also shown) (units in the table are mg / L. ”, And then cultured with shaking at 30 ° C. and 60 rpm. The number of general bacteria in the test water was measured according to JIS K0101 63.2, 24, 72 and 168 hours after the start of culture.

測定結果を表4に併せて示す(表中”<10”は10個/mL未満であることを示す)。なお、試験開始時の試験水の一般細菌数は78000個/mLであった。   The measurement results are also shown in Table 4 (“<10” in the table indicates less than 10 / mL). The number of general bacteria in the test water at the start of the test was 78000 / mL.

Figure 2010235509
Figure 2010235509

Figure 2010235509
Figure 2010235509

表4により本発明にかかる微生物防除剤が、極めて高い相乗的な微生物防除性能を有していること、さらに、その高い微生物防除性能が長時間維持されることが判る。一方、従来から汎用されている5−クロロ−2−メチル−4−イソチアゾリン−3−オンとカチオンポリマーとの併用の場合、殺菌効果に即効性があり、相乗的な作用も認められるものの、効果に持続性がなく、1週間(168時間)経過後には細菌数の上昇が認められた。   Table 4 shows that the microbial control agent according to the present invention has a very high synergistic microbial control performance, and that the high microbial control performance is maintained for a long time. On the other hand, the combined use of 5-chloro-2-methyl-4-isothiazolin-3-one and a cationic polymer that have been widely used in the past has an immediate effect on the bactericidal effect and a synergistic effect is also recognized. No increase in the number of bacteria was observed after one week (168 hours).

Claims (2)

ポリ[オキシエチレン(ジメチルイミニオ)エチレン(ジメチルイミニオ)エチレンジクロライド]、及び/または、ポリ(2−ヒドロキシプロピルジメチルアンモニウムクロライド)と、
2−メチル−4−イソチアゾリン−3−オンと、
を有効成分として含有することを特徴とする微生物防除剤。
Poly [oxyethylene (dimethyliminio) ethylene (dimethyliminio) ethylene dichloride] and / or poly (2-hydroxypropyldimethylammonium chloride);
2-methyl-4-isothiazolin-3-one;
A microorganism control agent characterized by comprising as an active ingredient.
ポリ[オキシエチレン(ジメチルイミニオ)エチレン(ジメチルイミニオ)エチレンジクロライド]、及び/または、ポリ(2−ヒドロキシプロピルジメチルアンモニウムクロライド)と、
2−メチル−4−イソチアゾリン−3−オンと、
を有効成分として水系水に添加することを特徴とする微生物防除方法。
Poly [oxyethylene (dimethyliminio) ethylene (dimethyliminio) ethylene dichloride] and / or poly (2-hydroxypropyldimethylammonium chloride);
2-methyl-4-isothiazolin-3-one;
A method for controlling microorganisms, which comprises adding as an active ingredient to aqueous water.
JP2009085033A 2009-03-31 2009-03-31 Microbial control agent and microorganism control method Active JP5356884B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2009085033A JP5356884B2 (en) 2009-03-31 2009-03-31 Microbial control agent and microorganism control method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2009085033A JP5356884B2 (en) 2009-03-31 2009-03-31 Microbial control agent and microorganism control method

Related Child Applications (1)

Application Number Title Priority Date Filing Date
JP2013101387A Division JP5547833B2 (en) 2013-05-13 2013-05-13 Microbial control agent and microorganism control method

Publications (2)

Publication Number Publication Date
JP2010235509A true JP2010235509A (en) 2010-10-21
JP5356884B2 JP5356884B2 (en) 2013-12-04

Family

ID=43090197

Family Applications (1)

Application Number Title Priority Date Filing Date
JP2009085033A Active JP5356884B2 (en) 2009-03-31 2009-03-31 Microbial control agent and microorganism control method

Country Status (1)

Country Link
JP (1) JP5356884B2 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012214388A (en) * 2011-03-31 2012-11-08 Aquas Corp Biofilm peeling agent, and method for peeling the biofilm
JP2015193577A (en) * 2014-03-31 2015-11-05 アクアス株式会社 Microorganism control agent composition

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02138103A (en) * 1988-11-04 1990-05-28 Buckman Lab Internatl Inc Composition for prevention of proliferation of microbes
JPH05246807A (en) * 1991-11-14 1993-09-24 Rohm & Haas Co Microbicidal composition comprising 3-isothiazolone and polycation
JP2004507475A (en) * 2000-08-31 2004-03-11 トール ゲーエムベーハー Synergistic biocide composition comprising 2-methylisothiazolin-3-one
JP2004099529A (en) * 2002-09-10 2004-04-02 Nagase Chemtex Corp Antimicrobial agent composition
JP2007022949A (en) * 2005-07-14 2007-02-01 Kemikurea:Kk New microbicidal composition
JP2009155220A (en) * 2007-12-25 2009-07-16 Aquas Corp Algae inhibitor and method for inhibiting algae

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02138103A (en) * 1988-11-04 1990-05-28 Buckman Lab Internatl Inc Composition for prevention of proliferation of microbes
JPH05246807A (en) * 1991-11-14 1993-09-24 Rohm & Haas Co Microbicidal composition comprising 3-isothiazolone and polycation
JP2004507475A (en) * 2000-08-31 2004-03-11 トール ゲーエムベーハー Synergistic biocide composition comprising 2-methylisothiazolin-3-one
JP2004099529A (en) * 2002-09-10 2004-04-02 Nagase Chemtex Corp Antimicrobial agent composition
JP2007022949A (en) * 2005-07-14 2007-02-01 Kemikurea:Kk New microbicidal composition
JP2009155220A (en) * 2007-12-25 2009-07-16 Aquas Corp Algae inhibitor and method for inhibiting algae

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012214388A (en) * 2011-03-31 2012-11-08 Aquas Corp Biofilm peeling agent, and method for peeling the biofilm
JP2015193577A (en) * 2014-03-31 2015-11-05 アクアス株式会社 Microorganism control agent composition

Also Published As

Publication number Publication date
JP5356884B2 (en) 2013-12-04

Similar Documents

Publication Publication Date Title
JP6239643B2 (en) Synergistic disinfection enhancement
JP6239644B2 (en) disinfectant
JP5606820B2 (en) Treatment method for open circulating cooling water system
JP5227012B2 (en) Algae inhibitor and method for suppressing algae
JP2016077255A (en) Water mold pest control method in cultivation water
JP5095308B2 (en) Disinfectant composition
JP5770891B2 (en) Treatment method for open circulating cooling water system
US8778370B2 (en) Method and composition for inhibiting growth of microorganisms in industrial process waters in the presence of anionic anti-fouling additives
JP5356884B2 (en) Microbial control agent and microorganism control method
JP5186254B2 (en) Amoeba disinfectant and amoeba suppression method
JP5638825B2 (en) Algae inhibitor and method for suppressing algae
JP5928938B2 (en) Treatment method for open circulating cooling water system
JP6057526B2 (en) Treatment method for open circulating cooling water system
JP4733851B2 (en) Amoeba disinfectant, amoeba control method and legionella eradication method
JP7057091B2 (en) Treatment method of open circulation cooling water system
JP5547833B2 (en) Microbial control agent and microorganism control method
JP3814085B2 (en) Algae control agent and algae control method
JP5356877B2 (en) Granular green algae control agent and method for controlling granular green algae
JP5735328B2 (en) Microbial control agent and microorganism control method
JP4963055B2 (en) Disinfectant composition
JP2013158669A (en) Treatment method for open-circulating cooling water system
JP5596106B2 (en) Amoeba suppression method
JP5280896B2 (en) Microbial control agent and microorganism control method
JP5755923B2 (en) Biofilm peeling method
JP2008179571A (en) Microorganism-controlling agent and method for controlling microorganism

Legal Events

Date Code Title Description
A621 Written request for application examination

Free format text: JAPANESE INTERMEDIATE CODE: A621

Effective date: 20120203

A977 Report on retrieval

Free format text: JAPANESE INTERMEDIATE CODE: A971007

Effective date: 20130218

A131 Notification of reasons for refusal

Free format text: JAPANESE INTERMEDIATE CODE: A131

Effective date: 20130312

A521 Request for written amendment filed

Free format text: JAPANESE INTERMEDIATE CODE: A523

Effective date: 20130513

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: 20130813

A61 First payment of annual fees (during grant procedure)

Free format text: JAPANESE INTERMEDIATE CODE: A61

Effective date: 20130829

R150 Certificate of patent or registration of utility model

Ref document number: 5356884

Country of ref document: JP

Free format text: JAPANESE INTERMEDIATE CODE: R150

Free format text: JAPANESE INTERMEDIATE CODE: R150

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

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