JPH09295907A - Antimicrobial aqueous dispersion composition - Google Patents
Antimicrobial aqueous dispersion compositionInfo
- Publication number
- JPH09295907A JPH09295907A JP11256096A JP11256096A JPH09295907A JP H09295907 A JPH09295907 A JP H09295907A JP 11256096 A JP11256096 A JP 11256096A JP 11256096 A JP11256096 A JP 11256096A JP H09295907 A JPH09295907 A JP H09295907A
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- Prior art keywords
- dbnpa
- water
- suspension
- antibacterial composition
- added
- Prior art date
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は水懸濁状抗菌性組成
物に係り、特に工業用抗菌剤である２，２’−ジブロモ
−３−ニトリロプロピオンアミド（以下「ＤＢＮＰＡ」
と略記する。）の取扱い性等を改善した新規抗菌性組成
物に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an aqueous antibacterial composition, particularly 2,2'-dibromo-3-nitrilopropionamide (hereinafter "DBNPA") which is an industrial antibacterial agent.
Abbreviated. The present invention relates to a novel antibacterial composition having improved handleability and the like.
【０００２】[0002]
【従来の技術】従来、紙・パルプ工業における抄紙工程
や各種工業における冷却水系には、細菌や真菌によるス
ライムが発生し、製品の品質低下や生産効率の低下など
の障害を引き起こしている。2. Description of the Related Art Conventionally, slimes due to bacteria and fungi have been generated in papermaking processes in the paper and pulp industry and in cooling water systems in various industries, causing problems such as deterioration of product quality and production efficiency.
【０００３】そこで、これらの微生物による障害を防止
するために、各種の抗菌剤が使用されている。特にＤＢ
ＮＰＡは、殺菌力が強いことから広く使用されている
が、水に対する溶解度が２５℃で１．５ｇ−ＤＢＮＰＡ
／１００ｇ−水と比較的低いことから、従来、ＤＢＮＰ
Ａは一般的には親水性のアルコール系又はグリコール系
の有機溶剤或いはこれらの有機溶剤と水との混合溶剤に
溶解して使用されている。Therefore, various antibacterial agents are used in order to prevent the damages caused by these microorganisms. Especially DB
NPA is widely used because of its strong bactericidal activity, but its solubility in water is 1.5 g-DBNPA at 25 ° C.
/ 100g-Because of the relatively low water, DBNP
A is generally used by dissolving it in a hydrophilic alcohol-based or glycol-based organic solvent or a mixed solvent of these organic solvents and water.
【０００４】なお、ＤＢＮＰＡ以外の抗菌性化合物で
は、有機溶剤を用いない水懸濁状抗菌性組成物が公知で
ある。例えば、ＤＢＮＰＡ以外の、常温で固体の水難溶
性の抗菌性化合物について、平均粒子径を３μｍ以下の
微粉とすると共に、分散剤を使用して粘度２００〜５０
０ｃｐ（２０℃）の水懸濁液とすることにより、比較的
安定な水懸濁状抗菌性組成物が得られている。As the antibacterial compound other than DBNPA, an aqueous antibacterial composition which does not use an organic solvent is known. For example, with respect to antibacterial compounds that are solid at room temperature and hardly soluble in water other than DBNPA, fine powder having an average particle size of 3 μm or less is used, and a viscosity of 200 to 50 is obtained by using a dispersant.
By setting the water suspension to 0 cp (20 ° C.), a relatively stable water-suspended antibacterial composition is obtained.
【０００５】[0005]
【発明が解決しようとする課題】ＤＢＮＰＡを有機溶剤
に溶解させた抗菌性組成物は、引火性を有することか
ら、貯蔵又は取り扱い時に注意を要する上に、溶剤コス
トが高くつくという欠点がある。しかも、有機溶剤を用
いた場合であっても、ＤＢＮＰＡの溶解度は高くても３
０〜４０重量％と制限があり、抗菌性組成物の調製が容
易ではない。Since the antibacterial composition in which DBNPA is dissolved in an organic solvent has flammability, it has the drawbacks that caution is required during storage or handling and the cost of the solvent is high. Moreover, the solubility of DBNPA is high even when an organic solvent is used.
There is a limit of 0 to 40% by weight, and it is not easy to prepare an antibacterial composition.
【０００６】ＤＢＮＰＡを有機溶剤と水との混合溶剤に
溶解させたものは、上記引火性の低減とコスト削減のた
めに提案されたものであるが、この抗菌性組成物では、
ＤＢＮＰＡが水と反応して分解し、抗菌効果が低下する
という問題がある。A solution obtained by dissolving DBNPA in a mixed solvent of an organic solvent and water has been proposed to reduce the above flammability and cost, but in this antibacterial composition,
There is a problem that DBNPA reacts with water to decompose and the antibacterial effect decreases.
【０００７】一方、ＤＢＮＰＡを、従来のＤＢＮＰＡ以
外の抗菌性化合物と同様にして水懸濁液とした場合、Ｄ
ＢＮＰＡの比重が大きいために、粘度２００〜５００ｃ
ｐ（２０℃）程度の水懸濁状抗菌性組成物では、長期保
存時に層分離を起こし易い。On the other hand, when DBNPA is made into an aqueous suspension in the same manner as conventional antibacterial compounds other than DBNPA, D
Viscosity of 200-500c due to the large specific gravity of BNPA
A water-suspended antibacterial composition of about p (20 ° C.) easily causes layer separation during long-term storage.
【０００８】本発明は上記従来の問題点を解決し、抗菌
性化合物としてＤＢＮＰＡを用いた水懸濁状抗菌性組成
物であって、層分離等の問題がなく、取り扱い性に優れ
た水懸濁状抗菌性組成物を提供することを目的とする。The present invention is a water-suspended antibacterial composition which solves the above-mentioned conventional problems and uses DBNPA as an antibacterial compound, which is free from problems such as layer separation and is easy to handle. It is intended to provide a turbid antibacterial composition.
【０００９】[0009]
【課題を解決するための手段】本発明の水懸濁状抗菌性
組成物は、２，２’−ジブロモ−３−ニトリロプロピオ
ンアミドを水に懸濁させると共に、増粘剤を添加して粘
度を６００〜３０００ｃｐ（２０℃）の範囲としたこと
を特徴とする。A water-suspended antibacterial composition of the present invention is prepared by suspending 2,2'-dibromo-3-nitrilopropionamide in water and adding a thickener to increase the viscosity. Is in the range of 600 to 3000 cp (20 ° C.).
【００１０】ＤＢＮＰＡは下記の構造式を有する。DBNPA has the following structural formula:
【００１１】[0011]
【化１】 Embedded image
【００１２】本発明の水懸濁状抗菌性組成物は、有機溶
剤を用いることなくＤＢＮＰＡを水に懸濁したものであ
るため、安価で引火性がなく、しかも、粘度が高いため
ＤＢＮＰＡの沈降分離の問題もなく、ＤＢＮＰＡを８０
重量％程度の高濃度とすることができる。また、本発明
の水懸濁状抗菌性組成物では、添加した増粘剤が、ＤＢ
ＮＰＡの水による分解を抑制し、水中でのＤＢＮＰＡの
化学的安定性に寄与していることが考えられる。更に薬
品の金属に対する腐食性が改善されるという効果も奏さ
れる。これは、有機溶剤中に比べ、水中の方が腐食の原
因となるＢｒがＤＢＮＰＡから解離し難いためと考えら
れる。Since the water-suspended antibacterial composition of the present invention is obtained by suspending DBNPA in water without using an organic solvent, it is inexpensive, has no flammability, and has a high viscosity. 80 DBNPA without separation problems
The concentration can be as high as about wt%. Further, in the water-suspended antibacterial composition of the present invention, the added thickener is DB
It is considered that it suppresses the decomposition of NPA by water and contributes to the chemical stability of DBNPA in water. Further, the effect of improving the corrosiveness of chemicals to metals is also exhibited. This is considered to be because Br, which causes corrosion, is less likely to be dissociated from DBNPA in water than in an organic solvent.
【００１３】このような本発明の水懸濁状抗菌性組成物
は、紙・パルプ工業における抄紙工程又は各種工業にお
ける冷却水系に用いる抗菌剤として有効である。The water-borne antibacterial composition of the present invention as described above is effective as an antibacterial agent used in a papermaking process in the paper / pulp industry or in a cooling water system in various industries.
【００１４】[0014]
【発明の実施の形態】以下に本発明の水懸濁状抗菌性組
成物を詳細に説明する。BEST MODE FOR CARRYING OUT THE INVENTION The water-suspended antibacterial composition of the present invention will be described in detail below.
【００１５】本発明の水懸濁状抗菌性組成物は、水にＤ
ＢＮＰＡを懸濁させると共に、増粘剤を添加して混合す
ることにより、所定の粘度の懸濁液とすることにより容
易に調製することができる。The water-suspended antibacterial composition of the present invention can be dissolved in water.
It can be easily prepared by suspending BNPA and adding and mixing a thickener to obtain a suspension having a predetermined viscosity.
【００１６】ＤＢＮＰＡの懸濁に当っては、水に、ＤＢ
ＮＰＡを添加して湿式粉砕するのが好ましい。この粉砕
はバッチ式，連続式の何れの方法で行っても良く、装置
としてはサンドミル，アトライター，ボールミルなどを
使用することができる。When suspending DBNPA, it is necessary to add DB to water.
It is preferable to add NPA and perform wet grinding. This pulverization may be performed by either a batch method or a continuous method, and a sand mill, an attritor, a ball mill or the like can be used as an apparatus.
【００１７】なお、ＤＢＮＰＡは、粉砕混合により粒子
径５μｍ以下の微粒子となっていることが懸濁液中のＤ
ＢＮＰＡ粒子の分散安定性の面で好ましい。It should be noted that DBNPA is formed into fine particles having a particle diameter of 5 μm or less by pulverization and mixing.
It is preferable in terms of dispersion stability of BNPA particles.
【００１８】本発明において、水懸濁状抗菌性組成物中
のＤＢＮＰＡ粒子の沈降防止を目的として添加される増
粘剤としては、高分子多糖類（ラムザンガム，キサンタ
ンガム，グアーガム等），セルロース誘導体（メチルセ
ルロース，エチルセルロース，ヒドロキシエチルセルロ
ース等）、合成高分子（ポリビニルアルコール，ポリビ
ニルピロリドン，ポリビニルメチルエーテル，ポリアク
リルアミド，カルボキシメチルセルロース等）、無機系
化合物（タルク，雲母，スメクタイト・クレー，ベント
ナイト，マグネシウム・アルミニウム・シリケート等）
が挙げられるが、これらに限定されるものではない。In the present invention, the thickener added for the purpose of preventing the precipitation of DBNPA particles in the water-suspended antibacterial composition includes polymeric polysaccharides (rhamzan gum, xanthan gum, guar gum, etc.), cellulose derivatives ( Methylcellulose, ethylcellulose, hydroxyethylcellulose, etc.), synthetic polymers (polyvinyl alcohol, polyvinylpyrrolidone, polyvinylmethyl ether, polyacrylamide, carboxymethylcellulose, etc.), inorganic compounds (talc, mica, smectite clay, bentonite, magnesium aluminum silicate) etc)
But are not limited to these.
【００１９】上記湿式粉砕に当っては、粉砕効率を向上
させると共に、粉砕後のＤＢＮＰＡ粒子の凝集を防ぐ目
的で、分散剤を添加するのが好ましい。従って、ＤＢＮ
ＰＡは、予め分散剤を溶解させた水に添加して粉砕混合
するのが好ましい。In the above wet pulverization, it is preferable to add a dispersant for the purpose of improving pulverization efficiency and preventing aggregation of DBNPA particles after pulverization. Therefore, DBN
It is preferable that PA is added to water in which a dispersant is dissolved in advance and pulverized and mixed.
【００２０】用いる分散剤としては、アニオン性，ノニ
オン性，カチオン性、又は両性の界面活性剤等が挙げら
れるが、特にアニオン性界面活性剤が好適である。分散
剤の添加量は、５重量％以下（純分としての水懸濁状抗
菌性組成物中の含有量）とするのが好ましい。Examples of the dispersant used include anionic, nonionic, cationic or amphoteric surfactants, and anionic surfactants are particularly preferable. The amount of the dispersant added is preferably 5% by weight or less (content in the water-suspended antibacterial composition as a pure content).
【００２１】なお、ＤＢＮＰＡと増粘剤は同時に添加し
ても良く、増粘剤添加後ＤＢＮＰＡを添加、或は、ＤＢ
ＮＰＡを添加後増粘剤を添加しても良い。DBNPA and the thickener may be added at the same time, or DBNPA may be added after the thickener has been added, or DBNPA may be added.
You may add a thickener after adding NPA.
【００２２】本発明において、このような増粘剤は、水
懸濁状抗菌性組成物の懸濁液の調製後の粘度が６００〜
３０００ｃｐ（２０℃）の範囲になるように添加する。
この粘度が６００ｃｐ未満であるとＤＢＮＰＡの比重が
大きいため、層分離を起こし易くなる。３０００ｃｐを
超える高粘度であると、長期保存時に増粘し易く、ま
た、ポンプ輸送が難しくなるなどの問題が生じる。従っ
て、懸濁液は、粘度が６００〜３０００ｃｐ（２０
℃）、特に８００〜１５００ｃｐ（２０℃）となるよう
に調製する。In the present invention, such a thickener has a viscosity of 600 to 600 after the suspension of the antibacterial composition in water is prepared.
Add so that it is in the range of 3000 cp (20 ° C.).
When this viscosity is less than 600 cp, the specific gravity of DBNPA is large, and thus layer separation easily occurs. If the viscosity is higher than 3000 cp, the viscosity tends to increase during long-term storage, and pumping becomes difficult. Therefore, the suspension has a viscosity of 600 to 3000 cp (20
C.), especially 800 to 1500 cp (20.degree. C.).
【００２３】また、本発明においては、得られる水懸濁
状抗菌性組成物に、別の機能を付与する目的で更に次の
ような添加剤を配合しても良い。ただし、以下に例示す
るものは配合し得る添加剤の一例であって、本発明にお
いて、用いる添加剤は何ら以下のものに限定されるもの
ではない。配合する添加剤が水難溶性である場合には、
水懸濁状にして添加しても良い。Further, in the present invention, the following additives may be further added to the resulting water-suspended antibacterial composition for the purpose of imparting another function. However, the following examples are examples of additives that can be blended, and the additives used in the present invention are not limited to the following. If the additive to be blended is poorly soluble in water,
It may be added in the form of a water suspension.
【００２４】腐食防止剤：トリルトリアゾール、ベンゾ
トリアゾール、メチルベンゾトリアゾール、モリブデン
酸、タングステン酸、ケイ酸、亜硝酸、２−ホスホノブ
タン−１，２，４−トリカルボン酸、ヒドロキシエチリ
デンジホスホン酸、ヘキサメタリン酸、トリポリリン
酸、正リン酸及びこれらの塩類、塩化亜鉛、塩酸酸性塩
化亜鉛、硫酸亜鉛、リグニンスルホン酸亜鉛、ヒドラジ
ン等 スケール防止剤：ポリアクリル酸、アクリル酸／ヒドロ
キシエチリデンメタアクリレートの共重合物、アクリル
酸／ヒドロキシエチリデンメタアクリレート／アクリル
酸メチルの共重合物、アクリル酸／アリルグリシジルエ
ーテル類の共重合物、アクリル酸／２−ヒドロキシ−３
−アリロキシ−１−プロパンスルホン酸の共重合物、ア
クリル酸／イソプレンスルホン酸の共重合物、アクリル
酸／ビニルスルホン酸、アクリル酸／アリルスルホン酸
の共重合物、マレイン酸又は無水マレイン酸／イソブチ
レンの共重合物、マレイン酸又は無水マレイン酸／スチ
レンスルホン酸の共重合物、マレイン酸又は無水マレイ
ン酸／アクリル酸の共重合物、マレイン酸又は無水マレ
イン酸／アクリレート酸の共重合物、マレイン酸又は無
水マレイン酸／２−アクリルアミド−２−メチルプロパ
ンスルホン酸の共重合物、マレイン酸又は無水マレイン
酸／アミレン酸の共重合物、マレイン酸又は無水マレイ
ン酸／アリル化蛍光物質（５−アリルベンゾスベレノー
ル等）の共重合物、ポリアクリルアミド、ポリイタコン
酸及びこれらの塩類等 ＤＢＮＰＡ以外の抗菌剤：ハロゲン化脂肪族ニトロアル
コール（２−ブロモ−２−ニトロ−１，３−プロパンジ
オール、２，２−ジブロモ−２−ニトロエタノール等）
及びこれらのエステル類、イソチアゾロン系化合物（５
−クロロ−２−メチル−４−イソチアゾリン−３−オ
ン、４，５−ジクロロ−２−オクチルイソチアゾリン−
３−オン、２−オクチルイソチアゾリン−３−オン、
１，２−ベンゾイソチアゾロン等）及びこれらの塩類又
は包接化合物、アルキレンビスチオシアネート（メチレ
ンビスチオシアネート等）、１，４−ビスブロモアセト
キシ−２−ブテン、ヘキサブロモジメチルスルホン、イ
ソフタロニトリル系化合物（５−クロロ−２，４，６−
トリフルオロイソフタロニトリル、テトラクロロイソフ
タロニトリル等）、ジメチルジチオカルバメート、４，
５−ジクロロ−１，２−ジチオール−３−オン、３，
３，４，４−テトラクロロテトラヒドロチオフェン−
１，１−ジオキシド、トリヨードアリルアルコール、ブ
ロモニトロスチレン、アルデヒド系化合物（グルタルア
ルデヒド、フタルアルデヒド、イソフタルアルデヒド、
テレフタルアルデヒド等）、ジクロログリオキシム、ベ
ンズアルドキシム系化合物（α−クロロベンズアルドキ
シムアセテート、α−クロロベンズアルドキシム等）、
５，５−ジメチルヒダントイン等 消泡剤：シリコン系、非シリコン系消泡剤等 防藻剤：２−メチルチオ−４−エチルアミノ−６−イソ
プロピルアミノ−Ｓ−トリアジン等 本発明の水懸濁状抗菌性組成物は、必要に応じて上述の
添加剤を添加して、例えば以下の配合で調製される。Corrosion inhibitors: tolyltriazole, benzotriazole, methylbenzotriazole, molybdic acid, tungstic acid, silicic acid, nitrous acid, 2-phosphonobutane-1,2,4-tricarboxylic acid, hydroxyethylidene diphosphonic acid, hexametaphosphoric acid , Tripolyphosphoric acid, orthophosphoric acid and salts thereof, zinc chloride, hydrochloric acid zinc chloride, zinc sulfate, zinc lignin sulfonate, hydrazine, etc. Scale inhibitor: polyacrylic acid, acrylic acid / hydroxyethylidene methacrylate copolymer, Acrylic acid / hydroxyethylidene methacrylate / methyl acrylate copolymer, acrylic acid / allyl glycidyl ether copolymer, acrylic acid / 2-hydroxy-3
-Aryloxy-1-propanesulfonic acid copolymer, acrylic acid / isoprene sulfonic acid copolymer, acrylic acid / vinyl sulfonic acid, acrylic acid / allyl sulfonic acid copolymer, maleic acid or maleic anhydride / isobutylene Copolymer, maleic acid or maleic anhydride / styrene sulfonic acid copolymer, maleic acid or maleic anhydride / acrylic acid copolymer, maleic acid or maleic anhydride / acrylate acid copolymer, maleic acid Or a maleic anhydride / 2-acrylamido-2-methylpropanesulfonic acid copolymer, maleic acid or maleic anhydride / amylenic acid copolymer, maleic acid or maleic anhydride / allylated fluorescent substance (5-allylbenzo (Suberenol, etc.) copolymer, polyacrylamide, polyitaconic acid and their salts Etc. DBNPA other antimicrobial agents: halogenated aliphatic nitro alcohol (2-bromo-2-nitro-1,3-propanediol, 2,2-dibromo-2-nitro ethanol, etc.)
And their esters, isothiazolone compounds (5
-Chloro-2-methyl-4-isothiazolin-3-one, 4,5-dichloro-2-octylisothiazolin-
3-one, 2-octylisothiazolin-3-one,
1,2-benzisothiazolone, etc.) and salts or inclusion compounds thereof, alkylenebisthiocyanate (methylenebisthiocyanate, etc.), 1,4-bisbromoacetoxy-2-butene, hexabromodimethylsulfone, isophthalonitrile compound ( 5-chloro-2,4,6-
Trifluoroisophthalonitrile, tetrachloroisophthalonitrile, etc.), dimethyldithiocarbamate, 4,
5-dichloro-1,2-dithiol-3-one, 3,
3,4,4-tetrachlorotetrahydrothiophene-
1,1-dioxide, triiodoallyl alcohol, bromonitrostyrene, aldehyde compounds (glutaraldehyde, phthalaldehyde, isophthalaldehyde,
Terephthalaldehyde, etc.), dichloroglyoxime, benzaldoxime compounds (α-chlorobenzaldoxime acetate, α-chlorobenzaldoxime, etc.),
5,5-Dimethylhydantoin, etc. Defoaming agent: Silicon-based, non-silicon-based defoaming agent, etc. Algal control agent: 2-methylthio-4-ethylamino-6-isopropylamino-S-triazine, etc. Water suspension of the present invention The antibacterial composition is prepared, for example, in the following formulation by adding the above-mentioned additives as necessary.
【００２５】配合割合（重量％：純分として） ＤＢＮＰＡ ：１〜８０ 分 散 剤 ：０．１〜５ 増 粘 剤 ：０．０１〜０．５ スケール防止剤：０〜５０ 腐食防止剤 ：０〜５０ ＤＢＮＰＡ以外の抗菌剤：０〜３０ 消 泡 剤 ：０〜１０ 防 藻 剤 ：０〜２０ このようにして得られる本発明の水懸濁状抗菌性組成物
は、紙・パルプ工業の抄紙工程や各種工業の冷却水系の
スライム防止を目的として、通常の場合、ＤＢＮＰＡ濃
度が０．１〜２５ｇ／ｍ3 となるように添加使用され
る。Blending ratio (wt%: as pure content) DBNPA: 1 to 80 minutes Dispersant: 0.1 to 5 Thickener: 0.01 to 0.5 Scale inhibitor: 0 to 50 Corrosion inhibitor: 0 -50 Antibacterial agent other than DBNPA: 0-30 Defoaming agent: 0-10 Antialgal agent: 0-20 The water-suspended antibacterial composition of the present invention thus obtained is a papermaking machine for paper and pulp industry. For the purpose of preventing slime in the cooling water system in the process and various industries, it is usually added and used so that the DBNPA concentration is 0.1 to 25 g / m 3 .
【００２６】[0026]
【実施例】以下に製造例、実施例及び比較例を挙げて本
発明をより具体的に説明するが、本発明はその要旨を超
えない限り以下の実施例に限定されるものではない。EXAMPLES The present invention will be more specifically described below with reference to production examples, examples and comparative examples, but the present invention is not limited to the following examples unless it exceeds the gist.
【００２７】なお、以下において粘度はＢ型回転粘度計
にて２０℃で測定した。In the following, the viscosity was measured at 20 ° C. with a B type rotational viscometer.
【００２８】製造例１：水懸濁状抗菌性組成物の製造 ステンレス製ビーカーに脱塩水３２．８５重量部と分散
剤として「ニューコール２４０」（日本乳化剤（株）
製：ポリプロピレングリコール硫酸エステルＮａ塩の３
０重量％水溶液）２．０重量部を添加し、撹拌して溶解
させた。これに、増粘剤としてラムザンガム（三晶
（株）製「Ｋ１Ａ１１２」）０．１５重量部を徐々に添
加し、添加終了後３０分間十分に撹拌してラムザンガム
を溶解させた。その後、ＤＢＮＰＡ６５重量部を添加
し、１０分間撹拌した。次に、直径１．３ｍｍのガラス
ビーズ１５０重量部を添加し、バッチ式卓上サンドミル
（カンペ社製）で４５分間撹拌（周速８ｍ／ｓｅｃ）し
て湿式粉砕した。粉砕後、ガラスビーズと懸濁液とをミ
ルセパレーターにより分離し、懸濁液Ａを得た。得られ
た懸濁液Ａは、ＤＢＮＰＡ含有率が６５重量％、粘度は
８６０ｃｐ（２０℃）、ＤＢＮＰＡの平均粒径は３．５
μｍであった。この懸濁液Ａは室温で１ケ月以上又は４
０℃で２週間以上安定で、ＤＢＮＰＡ含有率，粘度及び
ＤＢＮＰＡ粒子の凝集に関して変化がなく、層分離等も
引き起こすことなく安定に保存することができた。Production Example 1: Production of antibacterial composition in water suspension 32.85 parts by weight of deionized water and "Newcol 240" (Nippon Emulsifier Co., Ltd.) as a dispersant were added to a stainless steel beaker.
Made: polypropylene glycol sulfate Na salt 3
2.0 parts by weight of a 0% by weight aqueous solution was added and stirred to dissolve. To this, 0.15 parts by weight of rhamsan gum (“K1A112” manufactured by Sansho Co., Ltd.) as a thickener was gradually added and sufficiently stirred for 30 minutes after the addition was completed to dissolve the rhamzan gum. Then, 65 parts by weight of DBNPA was added and stirred for 10 minutes. Next, 150 parts by weight of glass beads having a diameter of 1.3 mm were added, and the mixture was wet-ground by stirring for 45 minutes with a batch-type tabletop sand mill (manufactured by Campe) (peripheral speed 8 m / sec). After crushing, the glass beads and the suspension were separated by a mill separator to obtain a suspension A. The obtained suspension A had a DBNPA content of 65% by weight, a viscosity of 860 cp (20 ° C.), and an average particle diameter of DBNPA of 3.5.
μm. This suspension A should be stored at room temperature for more than 1 month or 4
It was stable at 0 ° C. for 2 weeks or more, did not change in DBNPA content, viscosity and aggregation of DBNPA particles, and could be stably stored without causing layer separation.
【００２９】別に、比較の水懸濁状抗菌性組成物として
ラムザンガムの添加量を０．１重量部にしたこと以外は
上記と同様にして懸濁液を調製したところ、粘度が３７
３ｃｐ（２０℃）の懸濁液Ｂが得られた。この懸濁液Ｂ
は、室温で１ケ月後又は４０℃で２週間後には層分離を
起こし、製品安定性に問題があることが確認された。Separately, as a comparative water-suspended antibacterial composition, a suspension was prepared in the same manner as described above except that the amount of ramzan gum added was 0.1 parts by weight.
3 cp (20 ° C.) of suspension B was obtained. This suspension B
It was confirmed that, after 1 month at room temperature or 2 weeks at 40 ° C., layer separation occurred, and there was a problem in product stability.
【００３０】実施例１〜３，比較例１ ＜各種配合薬剤の調製及び安定性試験＞製造例１で製造
した懸濁液Ａを用いて表１に示す配合で薬剤を調製し
た。また、比較例としてプロピレングリコールにＤＢＮ
ＰＡを溶解させた薬剤を調製した。プロピレングリコー
ルに溶解させた場合は、低温時に析出が起こるので、Ｄ
ＢＮＰＡの添加量を２０重量％とした。各配合薬剤につ
いて、それぞれ４０℃及び室温で保存した場合の安定性
を調べ、結果を表１に示した。Examples 1 to 3 and Comparative Example 1 <Preparation of Various Compounded Drugs and Stability Test> The suspension A prepared in Preparation Example 1 was used to prepare the drugs shown in Table 1. Also, as a comparative example, DBN was added to propylene glycol.
A drug in which PA was dissolved was prepared. When dissolved in propylene glycol, precipitation occurs at low temperature, so D
The amount of BNPA added was 20% by weight. The stability of each compounded drug when stored at 40 ° C. and room temperature was examined, and the results are shown in Table 1.
【００３１】。表１に示す通り、いずれの薬剤も試験期
間は層分離等もなく安定であることが確認された。.. As shown in Table 1, it was confirmed that all the drugs were stable without separation of layers during the test period.
【００３２】[0032]
【表１】 [Table 1]
【００３３】＜薬剤の抗菌性試験＞Pseudomonas aerugi
nosaを用い、実施例１及び比較例１の薬剤の増殖阻止効
果を調べ、結果を表２に示した。<Antibacterial test of drug> Pseudomonas aerugi
The growth inhibitory effects of the drugs of Example 1 and Comparative Example 1 were examined using nosa, and the results are shown in Table 2.
【００３４】試験条件はｐＨ７の合成培地（リン酸一水
素カリウム７ｇ／Ｌ，リン酸二水素カリウム３ｇ／Ｌ，
クエン酸ナトリウム０．５ｇ／Ｌ，硫酸マグネシウム
０．１ｇ／Ｌ，硝酸ナトリウム１．２ｇ／Ｌ，１０％グ
ルコース２０ｍｌ／Ｌ）に前記菌を１０7 個／ｍｌとな
るように接種し、実施例１及び比較例１の薬剤を表２に
示すＤＢＮＰＡ濃度となるように添加し、３０℃で２４
時間振盪培養した。比較のため薬剤無添加のものについ
ても調べた。The test conditions were as follows: pH 7 synthetic medium (potassium monohydrogen phosphate 7 g / L, potassium dihydrogen phosphate 3 g / L,
Sodium citrate 0.5 g / L, magnesium sulfate 0.1 g / L, sodium nitrate 1.2 g / L, 10% glucose 20 ml / L) were inoculated with the above bacteria at 10 7 cells / ml, 1 and Comparative Example 1 were added so that the concentration of DBNPA shown in Table 2 was reached, and the mixture was added at 30 ° C. for 24 hours.
The cells were cultured with shaking for hours. For comparison, the samples without addition of chemicals were also examined.
【００３５】表２より、同一ＤＢＮＰＡ濃度において、
実施例１の薬剤は比較例１の薬剤と同等の増殖阻止効果
があることが確認された。From Table 2, at the same DBNPA concentration,
It was confirmed that the drug of Example 1 had the same growth inhibitory effect as the drug of Comparative Example 1.
【００３６】[0036]
【表２】 [Table 2]
【００３７】＜薬剤のＳＵＳ−３０４に対する腐食性試
験＞実施例１の薬剤と比較例１の薬剤各々５０ｍＬに、
ＳＵＳ−３０４製のテストピースを浸漬し、４０℃で１
４日間静置した後の腐食の状態を観察し、結果を表３に
示した。<Corrosion test of chemicals against SUS-304> 50 mL each of the chemicals of Example 1 and Comparative Example 1,
Immerse a test piece made of SUS-304, 1 at 40 ℃
The state of corrosion after standing for 4 days was observed, and the results are shown in Table 3.
【００３８】表３より明らかなように、比較例１の薬剤
は腐食が著しいのに対し、実施例１の薬剤では、防腐剤
を添加しないにも関わらず殆ど腐食が認められない。As is clear from Table 3, the chemical of Comparative Example 1 is significantly corroded, whereas the chemical of Example 1 shows almost no corrosion even though the preservative is not added.
【００３９】[0039]
【表３】 [Table 3]
【００４０】[0040]
【発明の効果】以上詳述した通り、本発明の水懸濁状抗
菌性組成物は、水にＤＢＮＰＡを分散させると共に増粘
剤を加えて所定の粘度とすることにより簡単に調製で
き、これによれば、 引火性がないため、貯蔵時や取り扱い時に制約を受
けることがない。 水へのＤＢＮＰＡの添加濃度を高くすることがで
き、所望の濃度のものを容易に調製できる。 分散媒コストが低減するため、安価に提供される。 層分離及びＤＢＮＰＡの化学的分解が防止され、長
期間安定に使用することができる。 防腐剤等を添加せずとも金属に対する腐食性が改善
され、配管や貯蔵槽の材質選定に苦慮する必要がない。 といった効果が奏され、本発明の水懸濁状抗菌性組成物
の工業的有用性は極めて大きい。As described in detail above, the water-suspended antibacterial composition of the present invention can be easily prepared by dispersing DBNPA in water and adding a thickener to give a predetermined viscosity. According to the report, since it is not flammable, it is not restricted during storage or handling. The concentration of DBNPA added to water can be increased, and a desired concentration can be easily prepared. Since the dispersion medium cost is reduced, it is provided at a low cost. The layer separation and the chemical decomposition of DBNPA are prevented, and it can be used stably for a long period of time. Corrosion to metals is improved without adding preservatives, so there is no need to worry about selecting materials for piping and storage tanks. Such effects are exhibited, and the industrial usefulness of the water-suspended antibacterial composition of the present invention is extremely large.
─────────────────────────────────────────────────────
─────────────────────────────────────────────────── ───
【手続補正書】[Procedure amendment]
【提出日】平成８年５月１０日[Submission date] May 10, 1996
【手続補正１】[Procedure amendment 1]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】００３８[Correction target item name] 0038
【補正方法】変更[Correction method] Change
【補正内容】[Correction contents]
【００３８】表３より明らかなように、比較例１の薬剤
は腐食が著しいのに対し、実施例１の薬剤では、防食剤
を添加しないにも関わらず殆ど腐食が認められない。As is apparent from Table 3, the agent of Comparative Example 1 whereas the corrosion that significant, the drug of Example 1, most corrosion is not observed despite no addition of anti-corrosion agent.
【手続補正２】[Procedure amendment 2]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】００４０[Correction target item name] 0040
【補正方法】変更[Correction method] Change
【補正内容】[Correction contents]
【００４０】[0040]
【発明の効果】以上詳述した通り、本発明の水懸濁状抗
菌性組成物は、水にＤＢＮＰＡを分散させると共に増粘
剤を加えて所定の粘度とすることにより簡単に調製で
き、これによれば、 引火性がないため、貯蔵時や取り扱い時に制約を受
けることがない。 水へのＤＢＮＰＡの添加濃度を高くすることがで
き、所望の濃度のものを容易に調製できる。 分散媒コストが低減するため、安価に提供される。 層分離及びＤＢＮＰＡの化学的分解が防止され、長
期間安定に使用することができる。 防食剤等を添加せずとも金属に対する腐食性が改善
され、配管や貯蔵槽の材質選定に苦慮する必要がない。 といった効果が奏され、本発明の水懸濁状抗菌性組成物
の工業的有用性は極めて大きい。As described in detail above, the water-suspended antibacterial composition of the present invention can be easily prepared by dispersing DBNPA in water and adding a thickener to give a predetermined viscosity. According to the report, since it is not flammable, it is not restricted during storage or handling. The concentration of DBNPA added to water can be increased, and a desired concentration can be easily prepared. Since the dispersion medium cost is reduced, it is provided at a low cost. The layer separation and the chemical decomposition of DBNPA are prevented, and it can be used stably for a long period of time. Without adding an anti-corrosion agent or the like improves the corrosion resistance to metals, there is no need to suffer from material selection of the piping and storage tanks. Such effects are exhibited, and the industrial usefulness of the water-suspended antibacterial composition of the present invention is extremely large.
Claims (1)
ピオンアミドを水に懸濁させると共に、増粘剤を添加し
て粘度を６００〜３０００ｃｐ（２０℃）の範囲とした
ことを特徴とする水懸濁状抗菌性組成物。1. A method of suspending 2,2′-dibromo-3-nitrilopropionamide in water and adding a thickener to adjust the viscosity to a range of 600 to 3000 cp (20 ° C.). A water-suspended antibacterial composition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11256096A JP3689971B2 (en) | 1996-05-07 | 1996-05-07 | Water suspension antibacterial composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11256096A JP3689971B2 (en) | 1996-05-07 | 1996-05-07 | Water suspension antibacterial composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH09295907A true JPH09295907A (en) | 1997-11-18 |
| JP3689971B2 JP3689971B2 (en) | 2005-08-31 |
Family
ID=14589740
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11256096A Expired - Fee Related JP3689971B2 (en) | 1996-05-07 | 1996-05-07 | Water suspension antibacterial composition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3689971B2 (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002079101A1 (en) * | 2001-04-02 | 2002-10-10 | Bromine Compounds Ltd. | Solid material dissolution apparatus |
| WO2002089578A1 (en) * | 2001-05-09 | 2002-11-14 | Toppan Forms Co., Ltd. | Microencapsulated antibacterial |
| WO2007081988A3 (en) * | 2006-01-11 | 2008-12-18 | Aurora Specialty Chemistries C | Stable dispersion of dbnpa in viscosified brine |
| US8628788B2 (en) | 2006-02-24 | 2014-01-14 | Bromine Compounds, Ltd. | Formulations containing a non-oxidative biocide and a source of active halogen and use thereof in water treatment |
| CN109418261A (en) * | 2017-08-25 | 2019-03-05 | 三博生化科技（上海）有限公司 | A kind of oxidation-reduction potential regulator, preparation method and its application |
-
1996
- 1996-05-07 JP JP11256096A patent/JP3689971B2/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002079101A1 (en) * | 2001-04-02 | 2002-10-10 | Bromine Compounds Ltd. | Solid material dissolution apparatus |
| WO2002089578A1 (en) * | 2001-05-09 | 2002-11-14 | Toppan Forms Co., Ltd. | Microencapsulated antibacterial |
| JPWO2002089578A1 (en) * | 2001-05-09 | 2004-08-19 | トッパン・フォームズ株式会社 | Microencapsulated antibacterial agent |
| WO2007081988A3 (en) * | 2006-01-11 | 2008-12-18 | Aurora Specialty Chemistries C | Stable dispersion of dbnpa in viscosified brine |
| US8628788B2 (en) | 2006-02-24 | 2014-01-14 | Bromine Compounds, Ltd. | Formulations containing a non-oxidative biocide and a source of active halogen and use thereof in water treatment |
| CN109418261A (en) * | 2017-08-25 | 2019-03-05 | 三博生化科技（上海）有限公司 | A kind of oxidation-reduction potential regulator, preparation method and its application |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3689971B2 (en) | 2005-08-31 |
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