JP2017186294A - Microorganism inhibitor composition and microorganism inhibition method - Google Patents
Microorganism inhibitor composition and microorganism inhibition method Download PDFInfo
- Publication number
- JP2017186294A JP2017186294A JP2016078488A JP2016078488A JP2017186294A JP 2017186294 A JP2017186294 A JP 2017186294A JP 2016078488 A JP2016078488 A JP 2016078488A JP 2016078488 A JP2016078488 A JP 2016078488A JP 2017186294 A JP2017186294 A JP 2017186294A
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- JP
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- Prior art keywords
- chloramine
- microorganism
- composition
- inhibitor composition
- acid
- Prior art date
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- 239000000203 mixture Substances 0.000 title claims abstract description 82
- 244000005700 microbiome Species 0.000 title claims abstract description 61
- 239000003112 inhibitor Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 31
- 230000005764 inhibitory process Effects 0.000 title abstract 3
- -1 bromine compound Chemical class 0.000 claims abstract description 41
- VDQQXEISLMTGAB-UHFFFAOYSA-N chloramine T Chemical compound [Na+].CC1=CC=C(S(=O)(=O)[N-]Cl)C=C1 VDQQXEISLMTGAB-UHFFFAOYSA-N 0.000 claims abstract description 36
- QDHHCQZDFGDHMP-UHFFFAOYSA-N Chloramine Chemical compound ClN QDHHCQZDFGDHMP-UHFFFAOYSA-N 0.000 claims abstract description 31
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052794 bromium Inorganic materials 0.000 claims abstract description 26
- 239000007800 oxidant agent Substances 0.000 claims description 29
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 23
- 239000000460 chlorine Substances 0.000 claims description 23
- 229910052801 chlorine Inorganic materials 0.000 claims description 23
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 claims description 22
- 230000000813 microbial effect Effects 0.000 claims description 19
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 16
- AMXOYNBUYSYVKV-UHFFFAOYSA-M lithium bromide Chemical compound [Li+].[Br-] AMXOYNBUYSYVKV-UHFFFAOYSA-M 0.000 claims description 10
- 230000002401 inhibitory effect Effects 0.000 claims description 9
- 241000894006 Bacteria Species 0.000 abstract description 22
- 241000589248 Legionella Species 0.000 abstract description 21
- 230000000694 effects Effects 0.000 abstract description 20
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Abstract
Description
本発明は、水系に添加使用される微生物抑制剤および微生物抑制方法に関し、特に、貯蔵安定性の高い酸化性の微生物抑制剤であって、水系に添加した際のバイオフィルムの成長抑制効果やレジオネラ属菌の除菌効果に優れた微生物抑制剤組成物、およびそれを用いた微生物抑制方法に関する。 The present invention relates to a microbial inhibitor and a microbial control method used in addition to an aqueous system, and in particular, is an oxidizing microbial inhibitor with high storage stability, and the biofilm growth inhibitory effect and Legionella when added to an aqueous system The present invention relates to a microbial inhibitor composition excellent in the sterilization effect of a genus and a microorganism control method using the same.
循環冷却水系、工業用工程水系などの各種の水系において、細菌類や真菌類、藻類などの微生物が原因で、さまざまな障害が発生する。例えば、開放循環式冷却水系においては、ズーグレア状細菌、糸状細菌、鉄バクテリア、イオウ細菌、硝化細菌、硫酸塩還元菌などの細菌類、ミズカビ、アオカビなどの真菌類、藍藻、緑藻、珪藻などの藻類が増殖し、これらの微生物を主体とし、土砂などの無機物や塵埃などが混ざりあって形成される軟泥状のスライムやスラッジが発生する。スライムやスラッジは、熱交換効率の低下や通水の悪化をもたらすばかりでなく、機器、配管などの局部腐食の原因となる。また、循環冷却水系や温泉、プール等で繁殖するレジオネラ属菌は人体の健康に影響を及ぼすので、それらの防止のために様々な技術的提案が行われている。 In various water systems such as circulating cooling water systems and industrial process water systems, various obstacles occur due to microorganisms such as bacteria, fungi and algae. For example, in an open-circulation cooling water system, bacteria such as zoom glial bacteria, filamentous bacteria, iron bacteria, sulfur bacteria, nitrifying bacteria, sulfate-reducing bacteria, fungi such as water mold and blue mold, cyanobacteria, green algae, diatoms, etc. Algae grow and soft mud-like slime and sludge are formed, which are mainly composed of these microorganisms and mixed with inorganic materials such as earth and sand and dust. Slime and sludge not only reduce heat exchange efficiency and water flow, but also cause local corrosion of equipment and piping. In addition, Legionella spp. That propagate in circulating cooling water systems, hot springs, pools, etc. have an impact on human health, and various technical proposals have been made to prevent them.
このような技術のうち、ハロゲン系酸化物による処理は、特開昭６４−１５２００号公報（特許文献１）、特開２０００−１４０８５７号公報（特許文献２）、特表２００３−５０３３２３号公報（特許文献３）や特表平１１−５０６１３９号公報（特許文献４）に開示されており、本出願人も特開２００９−１６０５０５号公報（特許文献５）で水系水におけるスライム抑制方法を提案している。 Among such techniques, treatment with a halogen-based oxide is disclosed in JP-A No. 64-15200 (Patent Document 1), JP-A No. 2000-140857 (Patent Document 2), JP-T-2003-503323 ( Patent Document 3) and Japanese Patent Application Laid-Open No. 11-506139 (Patent Document 4), and the present applicant also proposed a slime suppression method in aqueous water in JP 2009-160505 (Patent Document 5). ing.
この特許文献５により提案された方法は、低濃度のハロゲン系酸化物を含む薬剤を水系水に添加する技術であり、水系の金属材質に対する腐食を防止しながら極めて効果的に微生物の温床となるバイオフィルム（＝スライム）の抑制が可能となる。このように、ハロゲン系酸化物は細菌類の殺菌、バイオフィルムの成長抑制には極めて有効である。 The method proposed by Patent Document 5 is a technique of adding a chemical containing a low-concentration halogen-based oxide to aqueous water, and it becomes a very effective hotbed of microorganisms while preventing corrosion of the aqueous metal material. Biofilm (= slime) can be suppressed. Thus, halogen-based oxides are extremely effective for sterilizing bacteria and suppressing biofilm growth.
しかし、上記ハロゲン系酸化物は、優れた微生物抑制効果を示す一方、貯蔵安定性が悪く、これらを主成分とする微生物抑制剤をプラスチック容器などに充填して屋外などに保管、放置すると、酸化剤成分が徐々に分解し、微生物抑制性能が低下してしまうという課題を有している。 However, while the above halogen-based oxides exhibit excellent microbial control effects, they are poor in storage stability. If a microbial inhibitor containing these as a main component is filled in a plastic container or the like and stored or left outside, it is oxidized. There is a problem that the agent component is gradually decomposed and the microbial control performance is lowered.
上記課題に対し、本出願人は特開２０１４−１９６２６６号公報（特許文献６）で、分解を受けにくく、長期間安定してスライムコントロール性能を発揮することが可能な酸化性スライムコントロール剤組成物を提案している。 In response to the above problem, the present applicant is disclosed in Japanese Patent Application Laid-Open No. 2014-196266 (Patent Document 6), and is an oxidizing slime control agent composition that is difficult to be decomposed and can stably exhibit slime control performance for a long period of time. Has proposed.
この特許文献６により提案された組成物は、スライムコントロール性能を示す酸化性物質としてクロラミンＴおよびクロラミンＢから選択される少なくとも１種と、アゾール系化合物とを配合し、ｐＨを１０以上とするものであり、貯蔵安定性には優れるが、次亜塩素酸塩などと比較すると微生物を殺滅する力が相対的に弱く、効果面の向上が求められていた。 The composition proposed by Patent Document 6 is a composition in which at least one selected from chloramine T and chloramine B as an oxidizing substance exhibiting slime control performance and an azole compound are blended, and the pH is 10 or more. Although it is excellent in storage stability, it has a relatively weak ability to kill microorganisms compared to hypochlorite and the like, and an improvement in effectiveness has been demanded.
また、ハロゲン系酸化物には、実機においてレジオネラ属菌を十分に殺菌し、増殖を抑制することができないという問題点が存在する。すなわち、ハロゲン系酸化物は、実験室で培養したレジオネラ属菌に対しては優れた殺菌作用を示すが、実際の開放循環冷却水系等をハロゲン系酸化物で処理してみると、十分な殺菌、抑制効果が得られない場合が多く、驚くべきことに、遊離残留塩素濃度として２ｍｇ／Ｌを維持してもレジオネラ属菌を殺菌できない水系も存在する。引用文献６に記載の技術は、この点においても不十分であり、実機水において、レジオネラ属菌の除菌に有効な酸化性殺菌剤が求められていた。 Further, the halogen-based oxide has a problem that it cannot sufficiently sterilize Legionella spp. In an actual machine and cannot suppress growth. In other words, halogen-based oxides have an excellent bactericidal action against Legionella spp. Cultured in the laboratory, but when an actual open circulation cooling water system is treated with a halogen-based oxide, sufficient disinfection is achieved. In many cases, the inhibitory effect cannot be obtained. Surprisingly, there is an aqueous system in which Legionella spp. Cannot be sterilized even when the free residual chlorine concentration is maintained at 2 mg / L. The technique described in the cited document 6 is insufficient in this respect as well, and there has been a demand for an oxidative fungicide effective for eradication of Legionella in actual water.
本発明は、上記課題を解決する、すなわち、酸化性物質でありながら貯蔵安定性に優れ、しかも、細菌類、真菌類、藻類に加えて、アメーバ等の原生動物に対しても殺滅効果を示し、水系に添加した際のバイオフィルムの成長抑制効果やレジオネラ属菌の除菌効果に優れた微生物抑制剤組成物、および当該効果を有する微生物抑制方法を提供することを目的とする。 The present invention solves the above problems, that is, it is an oxidizing substance and excellent in storage stability, and also has a killing effect on protozoa such as amoeba in addition to bacteria, fungi and algae. It is an object of the present invention to provide a microbial inhibitor composition excellent in biofilm growth inhibitory effect and Legionella sterilizing effect when added to an aqueous system, and a microbial inhibitory method having the effect.
本発明者らは、上記の課題を解決すべく鋭意研究を重ねた結果、クロラミンＴおよびクロラミンＢから選択される少なくとも１種の酸化性物質と、臭素化合物とを水系中に共存させることで、従来技術からは想定できない優れた微生物抑制効果が得られることを見出し、本発明を完成するに至った。 As a result of intensive studies to solve the above problems, the present inventors have made a bromine compound coexist in an aqueous system with at least one oxidizing substance selected from chloramine T and chloramine B. The present inventors have found that an excellent microorganism suppressing effect that cannot be assumed from the prior art is obtained, and have completed the present invention.
すなわち、本発明の微生物抑制剤組成物は、請求項１に記載の通り、クロラミンＴおよびクロラミンＢから選択される少なくとも１種の酸化性物質と、臭素化合物の少なくとも１種とを含有することを特徴とする。 That is, the microorganism inhibitor composition of the present invention contains at least one oxidizing substance selected from chloramine T and chloramine B and at least one bromine compound as described in claim 1. Features.
また、本発明の微生物抑制剤組成物は、請求項２に記載の通り、請求項１に記載の微生物抑制剤組成物において、クロラミンＴおよびクロラミンＢから選択される少なくとも１種の酸化性物質の含有量が１質量％以上１５質量％以下であり、臭素化合物の含有量が０．５質量％以上３０質量％以下であることを特徴とする。 Moreover, the microorganism inhibitor composition of this invention is the microorganism inhibitor composition of Claim 1 as described in Claim 2, The at least 1 sort (s) of oxidizing substance selected from Chloramine T and Chloramine B of Claim 1 Content is 1 mass% or more and 15 mass% or less, Content of a bromine compound is 0.5 mass% or more and 30 mass% or less, It is characterized by the above-mentioned.
また、本発明の微生物抑制剤組成物は、請求項３に記載の通り、請求項１または請求項２に記載の微生物抑制剤組成物において、前記臭素化合物が臭化ナトリウム、臭化カリウム、および臭化リチウムから選択される少なくとも１種であることを特徴とする。 Further, the microorganism inhibitor composition of the present invention is the microorganism inhibitor composition according to claim 1 or 2, wherein the bromine compound is sodium bromide, potassium bromide, and It is at least one selected from lithium bromide.
本発明の微生物抑制方法は、請求項４に記載の通り、クロラミンＴおよびクロラミンＢから選択される少なくとも１種の酸化性物質と、臭素化合物の少なくとも１種とを水系に添加することを特徴とする。 The method for inhibiting microorganisms of the present invention is characterized in that, as described in claim 4, at least one oxidizing substance selected from chloramine T and chloramine B and at least one bromine compound are added to an aqueous system. To do.
また、本発明の微生物抑制方法は、請求項５に記載の通り、請求項４に記載の微生物抑制方法において、請求項１から請求項３の何れか１項に記載の微生物抑制剤組成物を水系に添加することを特徴とする。 Moreover, the microorganisms suppression method of this invention is the microorganisms suppression method of Claim 4, as described in Claim 5, The microorganisms inhibitor composition of any one of Claims 1-3 is used. It is added to an aqueous system.
また、本発明の微生物抑制方法は、請求項６に記載の通り、請求項４または請求項５に記載の微生物抑制方法において、水系中の結合留塩素濃度を、０．１ｍｇ／Ｌ以上、１００ｍｇ／Ｌ以下とすることを特徴とする。 Moreover, the microorganisms suppression method of this invention is the microorganisms suppression method of Claim 4 or Claim 5 as described in Claim 6, and the combined residual chlorine concentration in an aqueous system is 0.1 mg / L or more and 100 mg. / L or less.
本発明の微生物抑制剤組成物は、クロラミンＴおよびクロラミンＢから選択される少なくとも１種の酸化性物質と、臭素化合物の少なくとも１種とを含有し、貯蔵安定性に優れた酸化性殺菌剤であるとともに、本微生物抑制剤組成物を水系に適用することで、優れたバイオフィルムの成長抑制効果やレジオネラ属菌の除菌効果を示すものである。 The microorganism inhibitor composition of the present invention is an oxidizing fungicide containing at least one oxidizing substance selected from chloramine T and chloramine B and at least one bromine compound, and having excellent storage stability. In addition, by applying the present microbial inhibitor composition to an aqueous system, an excellent biofilm growth inhibitory effect and a sterilizing effect of Legionella spp. Are exhibited.
また、クロラミンＴおよびクロラミンＢから選択される少なくとも１種の酸化性物質の含有量を１質量％以上１５質量％以下、臭素化合物の含有量を０．５質量％以上３０質量％以下とし、該臭素化合物として臭化ナトリウム、臭化カリウム、臭化リチウムから選択される少なくとも１種を用いることで、組成物の貯蔵安定性をより確実なものとすることができる。 Further, the content of at least one oxidizing substance selected from chloramine T and chloramine B is 1% by mass to 15% by mass, and the bromine compound content is 0.5% by mass to 30% by mass, By using at least one selected from sodium bromide, potassium bromide and lithium bromide as the bromine compound, the storage stability of the composition can be made more reliable.
また、本発明の微生物抑制方法は、水系にクロラミンＴおよびクロラミンＢから選択される少なくとも１種の酸化性物質と臭素化合物の少なくとも１種とを添加することで、細菌類、真菌類、藻類に加えて、アメーバ等の原生動物に対しても殺滅効果を示し、バイオフィルムの成長抑制効果やレジオネラ属菌の除菌効果を得ることが可能となる。この際、水系中の結合留塩素濃度を０．１ｍｇ／Ｌ以上１００ｍｇ／Ｌ以下とすると、微生物の抑制効果を確実なものとするとともに、酸化性物質による水系内の金属材料の腐食を最小限に抑制することが可能となる。 In addition, the method for inhibiting microorganisms of the present invention adds at least one oxidizing substance selected from chloramine T and chloramine B and at least one bromine compound to an aqueous system, whereby bacteria, fungi and algae are added. In addition, it exhibits a killing effect on protozoa such as amoeba, and it is possible to obtain a biofilm growth suppression effect and a Legionella eradication effect. At this time, if the concentration of bonded residual chlorine in the aqueous system is 0.1 mg / L or more and 100 mg / L or less, the effect of suppressing microorganisms is ensured and the corrosion of the metal material in the aqueous system by the oxidizing substance is minimized. Can be suppressed.
本発明の微生物抑制剤組成物は、クロラミンＴおよびクロラミンＢから選択される少なくとも１種の酸化性物質と、臭素化合物の少なくとも１種とを含有する微生物抑制剤組成物である。 The microorganism inhibitor composition of the present invention is a microorganism inhibitor composition containing at least one oxidizing substance selected from chloramine T and chloramine B and at least one bromine compound.
本発明で酸化性物質として用いるクロラミンＴとは、ＩＵＰＡＣ名：Ｎ−クロロ−４−メチルベンゼンスルホンアミドのことであり、クロラミンＢとは、ＩＵＰＡＣ名：Ｎ−クロロベンゼンスルホンアミドのことである。通常、ナトリウム塩の水和物の形で市販されているが、水に溶けて酸化力を示し、微生物抑制効果が得られるものであれば、塩の種類を問わず本発明に含まれる。このような塩として、ナトリウム塩の他に、リチウム塩、カリウム塩等が挙げられる。クロラミンＴおよびクロラミンＢは、水中で結合残留塩素として酸化力を示し、各種微生物の殺滅、増殖抑制に寄与する。市販のクロラミンＴおよびクロラミンＢを水系に添加した場合、何れも固形分としての水系への添加濃度に対して約４分の１の濃度の結合塩素が水中に検出されるようになる。すなわち、酸化力の消費、分解を無視した場合、クロラミンＴ、クロラミンＢの４ｍｇ／Ｌ水溶液の示す結合残留塩素濃度は１ｍｇ／Ｌである。 Chloramine T used as an oxidizing substance in the present invention is IUPAC name: N-chloro-4-methylbenzenesulfonamide, and chloramine B is IUPAC name: N-chlorobenzenesulfonamide. Usually, it is commercially available in the form of a hydrate of sodium salt, but it is included in the present invention regardless of the type of salt, as long as it dissolves in water and exhibits oxidizing power and provides a microbial control effect. Examples of such salts include lithium salts and potassium salts in addition to sodium salts. Chloramine T and chloramine B exhibit oxidizing power as bound residual chlorine in water and contribute to the killing and growth suppression of various microorganisms. When commercially available chloramine T and chloramine B are added to the aqueous system, bound chlorine having a concentration of about one-fourth of the concentration added to the aqueous system as a solid content is detected in the water. That is, when igniting power consumption and decomposition are ignored, the 4 mg / L aqueous solution of chloramine T and chloramine B has a combined residual chlorine concentration of 1 mg / L.
本発明の微生物抑制剤組成物は、前記クロラミンＴおよびクロラミンＢから選択される少なくとも１種の酸化性物質を含有する。酸化性物質としてクロラミンＴやクロラミンＢを用いることで、次亜塩素酸ナトリウム等と比較して貯蔵安定性が格段に向上する。好ましい酸化性物質は、入手しやすさの点でクロラミンＴである。 The microorganism inhibitor composition of the present invention contains at least one oxidizing substance selected from the above chloramine T and chloramine B. By using chloramine T or chloramine B as the oxidizing substance, the storage stability is remarkably improved as compared with sodium hypochlorite or the like. A preferred oxidizing material is chloramine T in terms of availability.
本発明の微生物抑制剤組成物中のクロラミンＴまたはクロラミンＢの少なくとも１種の含有量は、通常は概略０．５質量％以上、２０質量％以下程度であるが、１質量％以上１５質量％以下とするのが、組成物が安定で、長期間放置しても析出物等が発生しない点で好ましい。 The content of at least one of chloramine T or chloramine B in the microorganism inhibitor composition of the present invention is usually about 0.5% by mass or more and 20% by mass or less, but 1% by mass or more and 15% by mass. The following is preferable because the composition is stable and precipitates are not generated even when left for a long period of time.
本発明の微生物抑制剤組成物は、臭素化合物を含有する。臭素化合物としては、臭化ナトリウム、臭化カリウム、臭化リチウム、臭化カルシウム、臭化マグネシウムおよび臭化アンモニウム等が挙げられる。これらのうち、臭化ナトリウム、臭化カリウム、臭化リチウムを用いるのが貯蔵安定性の点で好ましく、臭化カリウムを用いると特に貯蔵安定性に優れた製剤が可能となる。 The microorganism inhibitor composition of the present invention contains a bromine compound. Examples of the bromine compound include sodium bromide, potassium bromide, lithium bromide, calcium bromide, magnesium bromide and ammonium bromide. Of these, sodium bromide, potassium bromide, and lithium bromide are preferably used from the viewpoint of storage stability. When potassium bromide is used, a preparation having particularly excellent storage stability is possible.
本発明の微生物抑制剤組成物中の臭素化合物の含有量は、通常は概略０．２質量％以上３５質量％以下程度であるが、０．５質量％以上３０質量％以下とするのが、組成物が安定で、長期間放置しても析出物等が発生しない点で好ましい。 The content of the bromine compound in the microorganism inhibitor composition of the present invention is generally about 0.2% by mass or more and 35% by mass or less, but 0.5% by mass or more and 30% by mass or less. It is preferable in that the composition is stable and precipitates do not occur even when left for a long period of time.
本発明の微生物抑制剤組成物の製造方法は、特に限定されない。例えば、予め臭素化合物の少なくとも１種、及び必要によりその他の添加剤を加えた水溶液に、クロラミンＴおよびクロラミンＢから選択される少なくとも１種の酸化性物質を添加混合する方法が挙げられる。 The manufacturing method of the microorganism inhibitor composition of this invention is not specifically limited. For example, there is a method in which at least one oxidizing substance selected from chloramine T and chloramine B is added to and mixed with an aqueous solution in which at least one bromine compound and, if necessary, other additives are added.
本発明の微生物抑制剤組成物は、製造の容易性や酸化性物質の安定性を確保するために組成物のｐＨを９．５以上とするのが好ましい。より好ましい組成物のｐＨは１０．０以上であり、さらに好ましくは１１．５以上、１３．５未満である。組成物のｐＨ調整に用いるｐＨ調整剤としては、一般的なアルカリ剤が使用でき、水酸化ナトリウム、水酸化カリウム、水酸化リチウム等が好適に使用される。 In the microorganism inhibitor composition of the present invention, the pH of the composition is preferably 9.5 or more in order to ensure the ease of production and the stability of the oxidizing substance. The pH of the more preferable composition is 10.0 or more, More preferably, it is 11.5 or more and less than 13.5. As a pH adjuster used for adjusting the pH of the composition, a general alkali agent can be used, and sodium hydroxide, potassium hydroxide, lithium hydroxide, and the like are preferably used.
本発明の微生物抑制方法は、微生物抑制対象の水系に対して、クロラミンＴおよびクロラミンＢから選択される少なくとも１種の酸化性物質と、臭素化合物の少なくとも１種とを添加する方法である。臭素化合物を添加することで、クロラミンＴおよびクロラミンＢから選択される少なくとも１種の酸化性物質のみを添加した場合と比較して、微生物抑制効果が格段に向上する。 The microorganism suppression method of the present invention is a method in which at least one oxidizing substance selected from chloramine T and chloramine B and at least one bromine compound are added to an aqueous system targeted for microorganism suppression. By adding a bromine compound, the effect of suppressing microorganisms is significantly improved as compared with the case where only at least one oxidizing substance selected from chloramine T and chloramine B is added.
本発明の微生物抑制方法において、クロラミンＴおよびクロラミンＢから選択される少なくとも１種の酸化性物質と、臭素化合物の少なくとも１種、それぞれの水系への添加方法に特に制限はなく、酸化性物質と臭素化合物を別々に添加しても同時に添加しても、本発明の微生物抑制剤組成物のように予め両者を混合し、一剤化したものを添加しても良い。ここで、一剤化したものを水系に添加すると、個別に添加した場合と比較して微生物抑制効果が向上するので、より好ましい形態である。 In the method for suppressing microorganisms of the present invention, there is no particular limitation on the method of adding at least one oxidizing substance selected from chloramine T and chloramine B and at least one bromine compound to each aqueous system. The bromine compound may be added separately or simultaneously, or a mixture obtained by mixing both in advance as in the microbial inhibitor composition of the present invention may be added. Here, it is a more preferable mode to add a monolithic product to an aqueous system because the effect of suppressing microorganisms is improved as compared with the case where it is added individually.
本発明の微生物抑制方法では、水系中の結合留塩素濃度が０．１ｍｇ／Ｌ以上１００ｍｇ／Ｌ以下となるようにクロラミンＴおよびクロラミンＢから選択される少なくとも１種の酸化性物質の添加量を調整する。結合残留塩素濃度が０．１ｍｇ／Ｌ未満だと所望の微生物抑制効果が得られず、１００ｍｇ／Ｌを超えて添加すると、酸化性物質による水系内の金属材料の腐食リスクが高まるので好ましくない。より好ましい結合塩素濃度は、０．５ｍｇ／Ｌ以上２０ｍｇ／Ｌ以下である。なお、水系中の結合残留塩素濃度の測定は、常法に従って行えばよく、例えば、ＪＩＳ Ｋ０１０１ ２８項に記載された方法を適宜採用することができる。 In the microorganism control method of the present invention, the amount of at least one oxidizing substance selected from chloramine T and chloramine B is adjusted so that the bound chlorine content in the aqueous system is 0.1 mg / L or more and 100 mg / L or less. adjust. If the combined residual chlorine concentration is less than 0.1 mg / L, the desired effect of inhibiting microorganisms cannot be obtained, and if it exceeds 100 mg / L, the corrosion risk of the metallic material in the aqueous system due to the oxidizing substance is increased, which is not preferable. A more preferable combined chlorine concentration is 0.5 mg / L or more and 20 mg / L or less. In addition, what is necessary is just to perform the measurement of the joint residual chlorine density | concentration in an aqueous system in accordance with a conventional method, For example, the method described in JIS K0101 28 item | term can be employ | adopted suitably.
本発明の微生物抑制方法において、臭素化合物の水系への添加量は、クロラミンＴおよびクロラミンＢから選択される少なくとも１種の酸化性物質の水系への添加量を１としたときに、重量比で０．２から５の範囲とするのが良好な微生物抑制効果を発揮させる上で好ましい。 In the method for inhibiting microorganisms of the present invention, the amount of bromine compound added to the aqueous system is 1 by weight, where the amount of at least one oxidizing substance selected from chloramine T and chloramine B is 1 A range of 0.2 to 5 is preferable in order to exert a good microorganism suppressing effect.
本発明の微生物抑制剤組成物には、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、従来から水処理用途で使用されている公知の防食剤、スケール防止剤、及びクロラミンＴおよびクロラミンＢ以外のスライムコントロール剤を適宜配合することができ、その場合も本発明に含まれる。 The microbial inhibitor composition of the present invention is a known anticorrosion agent and scale prevention conventionally used in water treatment applications for the purpose of further improving the properties of the composition as long as the effects of the present invention are not hindered. An agent and a slime control agent other than Chloramine T and Chloramine B can be added as appropriate, and such cases are also included in the present invention.
本発明の微生物抑制剤組成物に配合可能な防食剤としては、アゾール系化合物が好適である。アゾール系化合物としては、例えば、イミダゾール、ピラゾール、オキサゾール、チアゾール、トリアゾール、テトラゾールなどの単環式アゾール系化合物、ベンゾイミダゾール、ベンゾオキサゾール、ベンゾイソオキサゾール、ベンゾチアゾール、メルカプトベンゾイミダゾール、メルカプトメチルベンゾイミダゾール、メルカプトベンゾチアゾール、ベンゾトリアゾール、トリルトリアゾール、インダゾール、プリン、イミダゾチアゾール、ピラゾロオキサゾールなどの縮合多環式アゾール系化合物などや、さらにアゾール系化合物の中で塩を形成する化合物にあってはそれらの塩などを挙げることができる。これらのアゾール系化合物は、１種のみを配合しても、２種以上を組み合わせて配合しても構わない。好ましいアゾール系化合物は、酸化性物質の分解抑制効果が高い点で、ベンゾトリアゾールあるいはトリルトリアゾールである。 As an anticorrosive agent that can be blended in the microorganism inhibitor composition of the present invention, an azole compound is suitable. Examples of azole compounds include monocyclic azole compounds such as imidazole, pyrazole, oxazole, thiazole, triazole, tetrazole, benzimidazole, benzoxazole, benzisoxazole, benzothiazole, mercaptobenzimidazole, mercaptomethylbenzimidazole, Condensed polycyclic azole compounds such as mercaptobenzothiazole, benzotriazole, tolyltriazole, indazole, purine, imidazothiazole, and pyrazolooxazole, and other compounds that form salts among azole compounds A salt etc. can be mentioned. These azole compounds may be blended alone or in combination of two or more. A preferred azole compound is benzotriazole or tolyltriazole because it has a high effect of suppressing the decomposition of the oxidizing substance.
本発明の微生物抑制剤組成物に配合可能なアゾール系化合物以外の防食剤としては、例えば、リン酸またはその塩、ピロリン酸、トリポリリン酸、ヘキサメタリン酸等の重合リン酸またはその塩、亜鉛塩、モリブデン酸またはその塩、タングステン酸またはその塩、グルコン酸、クエン酸、酒石酸、フィチン酸、琥珀酸、乳酸等の有機カルボン酸またはその塩等を挙げることができる。 Examples of the anticorrosive agent other than the azole compound that can be blended in the microorganism inhibitor composition of the present invention include, for example, phosphoric acid or a salt thereof, polymerized phosphoric acid such as pyrophosphoric acid, tripolyphosphoric acid, hexametaphosphoric acid or a salt thereof, a zinc salt, Examples thereof include molybdic acid or a salt thereof, tungstic acid or a salt thereof, gluconic acid, citric acid, tartaric acid, phytic acid, succinic acid, and an organic carboxylic acid such as lactic acid or a salt thereof.
本発明の微生物抑制剤組成物に配合可能なスケール防止剤としては、例えば、２−ホスホノブタン−１，２，４−トリカルボン酸、１−ヒドロキシエチリデン−１，１−ジホスホン酸、アミノトリメチレンホスホン酸やこれらの水溶性塩などのホスホン酸類、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等のポリマー類、アクリル酸系重合体の次亜リン酸付加物等のホスフィノカルボン酸類、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等を挙げることができる。この中で、２−ホスホノブタン−１，２，４−トリカルボン酸又はその水溶性塩、マレイン酸、アクリル酸アルキル、ビニルアセテートの三元共重合体、ポリアクリル酸の次亜リン酸付加物、アクリル酸と２−アクリルアミド−２−メチルプロパンスルホン酸との共重合体の次亜リン酸付加物から選択される少なくとも１種のスケール防止剤を配合すると、配合したスケール防止剤による酸化性物質の分解がほとんどないので好ましい。 Examples of the scale inhibitor that can be incorporated into the microorganism inhibitor composition of the present invention include 2-phosphonobutane-1,2,4-tricarboxylic acid, 1-hydroxyethylidene-1,1-diphosphonic acid, and aminotrimethylenephosphonic acid. And phosphonic acids such as water-soluble salts thereof, acrylic acid-based, maleic acid-based, methacrylic acid-based, sulfonic acid-based, itaconic acid-based polymers, polymers such as isobutylene-based polymers and copolymers thereof, Examples include phosphinocarboxylic acids such as hypophosphorous acid adducts of acrylic acid polymers, aminocarboxylic acid compounds such as nitrilotriacetic acid, ethylenediaminetetraacetic acid, and diethylenetriaminepentaacetic acid. Among them, 2-phosphonobutane-1,2,4-tricarboxylic acid or its water-soluble salt, maleic acid, alkyl acrylate, terpolymer of vinyl acetate, hypophosphorous acid adduct of polyacrylic acid, acrylic When at least one scale inhibitor selected from a hypophosphorous acid adduct of a copolymer of an acid and 2-acrylamido-2-methylpropanesulfonic acid is blended, decomposition of the oxidizing substance by the blended scale inhibitor Is preferable because there is almost no.
本発明の微生物抑制剤組成物に配合可能なスライムコントロール剤としては、例えば、５−クロロ−２−メチル−４−イソチアゾリン−３−オン、２−メチル−４−イソチアゾリン−３−オン、１，２−ベンゾイソチアゾリン−３−オン、２−ｎ−オクチル−４−イソチアゾリン−３−オン等のイソチアゾリン系化合物、２，２−ジブロモ−２−ニトロエタノール、２−ブロモ−２−ニトロプロパン−１，３−ジオール等のブロモニトロアルコール系化合物、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、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等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］、（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）、ポリ（ヘキサメチレンビグアニド）などのヨーネンポリマー等のカチオン系化合物等を挙げることができる。 Examples of the slime control agent that can be blended in the microorganism inhibitor composition of the present invention include, for example, 5-chloro-2-methyl-4-isothiazolin-3-one, 2-methyl-4-isothiazolin-3-one, 1, Isothiazoline compounds such as 2-benzisothiazolin-3-one and 2-n-octyl-4-isothiazolin-3-one, 2,2-dibromo-2-nitroethanol, 2-bromo-2-nitropropane-1, Bromonitroalcohol compounds such as 3-diol, aldehyde compounds such as glutaraldehyde and phthalaldehyde, hydrogen peroxide, hydrazine, pyrithione compounds, dithiol compounds, thiocyanate compounds such as methylenebisthiocyanate, quaternary ammonium salt systems Compound, quaternary phosphonium salt compound, pyridinium salt compound Cation compounds such as ionene polymers such as poly [oxyethylene (dimethyliminio) ethylene (dimethyliminio) ethylene dichloride], (2-hydroxypropyldimethylammonium chloride), and poly (hexamethylenebiguanide). Can do.
以下に、本発明の微生物抑制剤組成物の実施例について具体的に説明するが、本発明はこれらによって限定されるものではない。 Examples of the microorganism inhibitor composition of the present invention will be specifically described below, but the present invention is not limited thereto.
＜貯蔵安定性の評価＞
表１に記載した、製剤例１〜１３の配合組成の組成物を調整した。なお、表中の配合組成欄の数値は、該当化合物の含有量（質量％）であり、残部は各組成物をｐＨ１３．０に調整するために使用した水酸化カリウムとイオン交換水である。また、配合組成欄に記載された略号等は以下の化合物を示す。
クロラミンＴ：Ｎ−クロロ−４−メチルベンゼンスルホンアミドナトリウム水和物
クロラミンＢ：Ｎ−クロロベンゼンスルホンアミドナトリウム水和物
ＮａＣｌＯ：５％次亜塩素酸ナトリウム溶液
ＳＡ：スルファミン酸
ＫＢｒ：臭化カリウム
ＮａＢｒ：臭化ナトリウム
<Evaluation of storage stability>
The composition of the formulation composition of the formulation examples 1-13 described in Table 1 was adjusted. In addition, the numerical value of the compounding composition column in a table | surface is content (mass%) of an applicable compound, and the remainder is potassium hydroxide and ion-exchange water which were used in order to adjust each composition to pH13.0. Moreover, the symbol etc. which were described in the compounding composition column show the following compounds.
Chloramine T: N-chloro-4-methylbenzenesulfonamide sodium hydrate Chloramine B: N-chlorobenzenesulfonamide sodium hydrate NaClO: 5% sodium hypochlorite solution SA: Sulfamic acid
KBr: potassium bromide NaBr: sodium bromide
上記１３種類の組成物を１００ｍＬ容のポリエチレン製白色細口ビンに１００ｍＬずつ分注し、薬剤タンク内の状況を再現するために、栓を緩くし通気可能な状態（半開放）で、４５℃の恒温庫内に２０日間静置した。２０日後に恒温庫から取り出し、各組成物について析出物の有無を確認したところ、全ての組成物に析出物は認められなかった。また、取り出した組成物について、酸化性物質が配合されていない製剤例１１を除き、組成物中の酸化力の測定を行い、各組成物の製剤直後の酸化力と比較して残存酸化力の割合（％）を求めた。結果を表１に合わせて記す。なお、組成物中の酸化力の測定は、ＪＩＳ Ｋ０１０１ ２８．３項記載のヨウ素滴定法に従って行った。 Dispense 100 mL of the above 13 types of compositions into a 100 mL polyethylene white narrow mouth bottle, and reproduce the situation in the drug tank. It left still for 20 days in a thermostat. After removing from the thermostat after 20 days and checking the presence or absence of precipitates for each composition, no precipitates were observed in all the compositions. Further, with respect to the extracted composition, the oxidizing power in the composition was measured except for Formulation Example 11 in which no oxidizing substance was blended, and the remaining oxidizing power was compared with the oxidizing power immediately after the preparation of each composition. The percentage (%) was determined. The results are shown in Table 1. The oxidizing power in the composition was measured according to the iodine titration method described in JIS K0101 28.3.
本発明の微生物抑制剤組成物である製剤例１〜７は、４５℃、半開放の条件でも２０日後の残存酸化力が９３％以上であった。クロラミンＴ（製剤例８）やクロラミンＢ（製剤例９）は、元々他の酸化性物質（製剤例１０〜１３）と比較して貯蔵安定性の良い組成物だが、臭素化合物として臭化カリウムや臭化ナトリウムを配合することで貯蔵安定性がさらに向上していることが理解される。 Formulation Examples 1 to 7, which are the microorganism inhibitor compositions of the present invention, had a remaining oxidizing power of 93% or more after 20 days even under the condition of 45 ° C. and half open. Chloramine T (Formulation Example 8) and Chloramine B (Formulation Example 9) are originally compositions having better storage stability than other oxidizing substances (Formulation Examples 10 to 13). It is understood that the storage stability is further improved by adding sodium bromide.
＜実験室で培養したレジオネラ属菌に対する殺菌力の評価＞
滅菌したつくば市水道水に、ＢＣＹＥα培地で２日間前培養したレジオネラ属菌（Legionella pneumophila ATCC33152株）を１ｍＬ当たりの菌数が２５万個となるように摂取し、これを滅菌済の５０ｍＬ容の培養フラスコに３０ｍＬずつ分取、表２に示す組成物を表２に示す濃度で添加した後、３０℃、６０ｒｐｍで往復振盪しながら２４時間放置し、２４時間後に各サンプル中のレジオネラ属菌数の測定を行った。結果を表２に合わせて記す。なお、表２中の残留塩素濃度は、各試験系における組成物添加直後の残留塩素濃度の測定値であり、比較例３は遊離残留塩素濃度、その他は結合残留塩素濃度の値である。
<Evaluation of bactericidal activity against Legionella spp. Cultured in the laboratory>
Legionella sp. (Legionella pneumophila ATCC33152 strain) pre-cultured in BCYEα medium for 2 days was ingested into sterilized Tsukuba City tap water so that the number of bacteria per mL was 250,000, and this was sterilized in a 50 mL volume. 30 mL each was aliquoted into a culture flask, the composition shown in Table 2 was added at the concentration shown in Table 2, and left for 24 hours with reciprocal shaking at 30 ° C. and 60 rpm. After 24 hours, the number of Legionella in each sample Was measured. The results are shown in Table 2. The residual chlorine concentration in Table 2 is a measured value of the residual chlorine concentration immediately after the addition of the composition in each test system, Comparative Example 3 is a free residual chlorine concentration, and the others are values of combined residual chlorine concentration.
実施例１〜１０の結果から、本発明の微生物抑制方法は、実験室で培養したレジオネラ属菌に対して遊離塩素（比較例３）と同等の優れた殺菌効果を示すことが理解される。一方、クロラミンＴやクロラミンＢを単独で作用させた場合（比較例１〜２）、レジオネラ属菌に対する殺菌効果は弱く、塩素化スルファミン酸（比較例４）、臭素化スルファミン酸（比較例５）、臭化カリウム（比較例６）は、実験室で培養したレジオネラ属菌に対しても、殺菌力を殆ど示さないことが判る。 From the results of Examples 1 to 10, it is understood that the microorganism suppression method of the present invention exhibits an excellent bactericidal effect equivalent to free chlorine (Comparative Example 3) against Legionella spp. Cultured in the laboratory. On the other hand, when chloramine T or chloramine B is allowed to act alone (Comparative Examples 1-2), the bactericidal effect against Legionella spp. Is weak, chlorinated sulfamic acid (Comparative Example 4), brominated sulfamic acid (Comparative Example 5). It can be seen that potassium bromide (Comparative Example 6) shows little bactericidal activity against Legionella spp. Cultured in the laboratory.
＜実機冷却水を用いた微生物抑制力の評価＞
茨城県内の某工場で稼働中の、薬剤処理をしていない冷却塔から採取した冷却水を用いて以下の実験を行った。５００ｍＬ容の滅菌済ポリプロピレン製容器に、冷却水を５００ｍＬずつ分取し、表３に示す組成物を表３に示す濃度で添加した後、室温で３日間静置し、３日後に各サンプル中の一般細菌数、従属栄養細菌数、レジオネラ属菌数、アメーバ数の測定を行った。結果を表４に記す。ここで、実施例１６は、クロラミンＴ単独の組成物である製剤例８と、臭化カリウム単独の組成物である製剤例１３とを別々に冷却水に添加して、冷却水中に両成分が存在するようにした試験例である。なお、表３中の残留塩素濃度は、各試験系における組成物添加直後の残留塩素濃度の測定値であり、比較例８は遊離残留塩素濃度、その他は結合残留塩素濃度の値である。また、表４中の初期微生物数の値は、組成物添加前の冷却水中の微生物数を測定した値である。
<Evaluation of microbial inhibitory power using actual cooling water>
The following experiment was conducted using cooling water collected from a cooling tower that is in operation at the Sakai Factory in Ibaraki Prefecture and is not treated with chemicals. In a 500 mL sterilized polypropylene container, 500 mL of cooling water is dispensed, and after adding the composition shown in Table 3 at the concentration shown in Table 3, it is allowed to stand at room temperature for 3 days, and in each sample after 3 days. General bacteria count, heterotrophic bacteria count, Legionella sp. Count, and amoeba count were measured. The results are shown in Table 4. Here, in Example 16, Formulation Example 8 which is a composition of chloramine T alone and Formulation Example 13 which is a composition of potassium bromide are separately added to cooling water, and both components are contained in cooling water. This is a test example that exists. The residual chlorine concentration in Table 3 is a measured value of the residual chlorine concentration immediately after the addition of the composition in each test system, Comparative Example 8 is a free residual chlorine concentration, and the others are values of combined residual chlorine concentration. Moreover, the value of the initial number of microorganisms in Table 4 is a value obtained by measuring the number of microorganisms in the cooling water before adding the composition.
実機冷却水中に生存する微生物を対象に試験を行うと、実験室で培養したレジオネラ属菌に対しては殺菌効果を示した遊離塩素（比較例８）による処理が、冷却水中に生育するレジオネラ属菌に対しては有効でないことが判る。 When the test was performed on microorganisms that survived in actual cooling water, treatment with free chlorine (Comparative Example 8) that showed bactericidal effect against Legionella spp. It turns out that it is not effective against bacteria.
一方、本発明の微生物抑制方法（実施例１１〜１６）は、冷却水中に生育するレジオネラ属菌に対しても強い殺菌効果を示すと共に、一般細菌、従属栄養細菌、アメーバ等の水中微生物の数を効果的に抑制できるので、水系におけるバイオフィルムの成長抑制や、レジオネラ属菌の除菌に有効である。また、実施例１６の結果から、本発明の微生物抑制方法は、クロラミンＴおよびクロラミンＢから選択される少なくとも１種の酸化性物質と、臭素化合物の少なくとも１種とを水系に別々に添加した場合でも、優れた微生物抑制効果を発揮することが明らかになった。 On the other hand, the microorganism control method of the present invention (Examples 11 to 16) shows a strong bactericidal effect against Legionella spp. Growing in cooling water, and the number of underwater microorganisms such as general bacteria, heterotrophic bacteria, and amoeba Therefore, it is effective for suppressing the growth of biofilms in water and eradicating Legionella spp. Moreover, from the result of Example 16, when the microorganisms suppression method of this invention adds at least 1 sort (s) of an oxidizing substance selected from chloramine T and chloramine B, and at least 1 sort (s) of a bromine compound separately to an aqueous system. However, it has been revealed that it exhibits an excellent microbial control effect.
＜実機冷却水系における微生物抑制力の評価＞
東京都内の某ビルで稼働中の薬剤処理を行っていない冷却塔において、製剤例８の組成物を冷却水中の結合残留塩素濃度が０．５ｍｇ／Ｌを維持するように添加する処理を１ヶ月間行い、その後、製剤例１の組成物を冷却水中の結合残留塩素濃度が０．５ｍｇ／Ｌを維持するように添加する処理を１ヶ月間行った。処理開始前、製剤例８による処理終了時、製剤例１による処理終了時に冷却塔充填剤の付着物の状況を観察するとともに、冷却水中の一般細菌数、従属栄養細菌数、レジオネラ属菌数、アメーバ数の測定を行った。結果を表５に記す。
<Evaluation of microbial control in actual cooling water system>
In a cooling tower that is not operating a chemical treatment in operation at a certain building in Tokyo, treatment for adding the composition of Formulation Example 8 so that the combined residual chlorine concentration in cooling water is maintained at 0.5 mg / L for one month Thereafter, the treatment of adding the composition of Formulation Example 1 so that the combined residual chlorine concentration in the cooling water was maintained at 0.5 mg / L was performed for one month. Before starting the treatment, at the end of the treatment according to Formulation Example 8, at the end of the treatment according to Formulation Example 1, observe the status of the adhering material on the cooling tower filler, and count the number of general bacteria, heterotrophic bacteria, Legionella spp. The number of amoeba was measured. The results are shown in Table 5.
クロラミンＴ単独の組成物である製剤例８を実機冷却水系で１ヶ月間継続使用した結果、薬剤処理を行っていないときに充填剤に付着していた細菌類と藍藻類主体のスライムはほぼ消滅したが、その効果は十分ではなく、新たに緑藻類主体のスライムが発生、付着してしまった。また、一般細菌数、従属栄養細菌数は、薬剤処理を行っていないときの１００分の１以下に減少したが、レジオネラ属菌やアメーバの数には変化が見られなかった。 As a result of continuous use of formulation example 8 which is a composition of chloramine T alone in the actual cooling water system for one month, bacteria and cyanobacteria-based slime adhering to the filler when chemical treatment is not performed are almost disappeared. However, the effect was not sufficient, and a new slime mainly composed of green algae was generated and adhered. Moreover, although the number of general bacteria and the number of heterotrophic bacteria decreased to 1/100 or less when the chemical treatment was not performed, there was no change in the number of Legionella bacteria or amoeba.
一方、本発明の組成物であるクロラミンＴに臭化カリウムを配合した製剤例１による処理を１ヶ月間継続した後は、冷却塔充填剤の付着物は殆どなくなり、レジオネラ属菌、アメーバ共に不検出になった。このように本発明の組成物は、実機冷却水系において優れたバイオフィルムの剥離および成長抑制効果、レジオネラ属菌の除菌効果を示すものである。 On the other hand, after the treatment by Formulation Example 1 in which potassium bromide was blended with chloramine T, which is the composition of the present invention, was continued for 1 month, there was almost no deposits on the cooling tower filler, and both Legionella sp. It became a detection. Thus, the composition of the present invention exhibits excellent biofilm detachment and growth suppression effects and legionella eradication effects in an actual cooling water system.
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