JP4815109B2 - Chlorine dioxide aqueous solution manufacturing method - Google Patents

Chlorine dioxide aqueous solution manufacturing method Download PDF

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JP4815109B2
JP4815109B2 JP2004226726A JP2004226726A JP4815109B2 JP 4815109 B2 JP4815109 B2 JP 4815109B2 JP 2004226726 A JP2004226726 A JP 2004226726A JP 2004226726 A JP2004226726 A JP 2004226726A JP 4815109 B2 JP4815109 B2 JP 4815109B2
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aqueous solution
chlorine dioxide
reaction chamber
container
acid
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JP2006044973A (en
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幸治 安部
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Taiko Pharmaceutical Co Ltd
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本発明は、亜塩素酸塩水溶液と酸とを反応させて二酸化塩素水溶液を生成可能な反応室と、前記反応室内の上部と反応室外とを連通可能な連通路とを備えた反応器を使用して二酸化塩素水溶液を製造する、二酸化塩素水溶液の製造方法に関する。   The present invention uses a reactor provided with a reaction chamber capable of reacting a chlorite aqueous solution with an acid to generate a chlorine dioxide aqueous solution, and a communication passage capable of communicating the upper portion of the reaction chamber with the outside of the reaction chamber. The present invention relates to a method for producing a chlorine dioxide aqueous solution.

強い酸化力と殺菌性とを備えた二酸化塩素は、常温ではガス状の物質であって、その水溶液は、殺菌や消毒用、脱臭用、漂白用などの用途に使用されている。   Chlorine dioxide having strong oxidizing power and bactericidal properties is a gaseous substance at room temperature, and its aqueous solution is used for sterilization, disinfection, deodorization, bleaching and the like.

上記の二酸化塩素水溶液の製造方法によれば、反応室と、その反応室内の上部と反応室外とを連通可能な連通路とを備えた反応器内で、高濃度の亜塩素酸塩水溶液と高濃度の酸とを反応させて、高濃度で生成効率の高い二酸化塩素水溶液が製造できる。しかしながら、製造時に水溶液中に溶解しなかった二酸化塩素は、悪臭を放ち、人体に対して有毒であり、さらに爆発性も有するガスになって連通路を通って反応室外に流出するので、従来は、希釈して反応させ、安全性及び取扱い性を重視している。しかしこのために低濃度でしかも反応効率も低く使用する薬品量も多く必要であった。   According to the above method for producing a chlorine dioxide aqueous solution, a high concentration chlorite aqueous solution and a high concentration chlorite aqueous solution can be obtained in a reactor equipped with a reaction chamber and a communication passage capable of communicating the upper portion of the reaction chamber with the outside of the reaction chamber. By reacting with a concentration of acid, a chlorine dioxide aqueous solution having a high concentration and high production efficiency can be produced. However, chlorine dioxide that did not dissolve in the aqueous solution at the time of production gives off a bad odor, is toxic to the human body, and further becomes explosive gas that flows out of the reaction chamber through the communication path. , Diluted and reacted, with emphasis on safety and handling. However, this requires a large amount of chemicals to be used at a low concentration and low reaction efficiency.

尚、この様な従来技術に関しては、当業者の間で広く知られているものであり、詳しく言及した特許文献などが無いため、先行技術文献を開示できない。   Such a prior art is widely known among those skilled in the art, and since there is no patent document or the like that is mentioned in detail, a prior art document cannot be disclosed.

この為、大気中に放散した二酸化塩素ガスによって、悪臭等の環境汚染を招来する虞がある。そこで、二酸化塩素ガスの発生を抑えるため、亜塩素酸塩水溶液及び酸をそれぞれ水で希釈して、それらを混合し、反応させて、二酸化塩素水溶液を製造する方法もあるが、この方法によれば、高濃度で生成効率の高い二酸化塩素水溶液が得られ難いという欠点がある。   For this reason, there is a possibility that environmental pollution such as bad odor may be caused by chlorine dioxide gas diffused into the atmosphere. Therefore, in order to suppress the generation of chlorine dioxide gas, there is a method in which a chlorite aqueous solution and an acid are diluted with water, mixed, and reacted to produce a chlorine dioxide aqueous solution. In other words, there is a drawback that it is difficult to obtain a chlorine dioxide aqueous solution having a high concentration and high production efficiency.

本発明は、上記実情に鑑みてなされたものであって、発生する二酸化塩素ガスによる環境汚染を防止すると同時に高濃度で生成効率の高い二酸化塩素水溶液が得られる方法を提供するものである。   The present invention has been made in view of the above circumstances, and provides a method for preventing environmental pollution by generated chlorine dioxide gas and at the same time obtaining a chlorine dioxide aqueous solution with high concentration and high production efficiency.

本発明の第１特徴構成は、亜塩素酸塩水溶液と酸とを反応させて二酸化塩素水溶液を生成可能な反応室と、前記反応室内の上部と前記反応室外とを連通可能な連通路とを備えた反応器を使用して二酸化塩素水溶液を製造する方法であって、前記反応器が、上面に取っ手部材を備える蓋部材と、内側に前記反応室を有し上部に開口部を有する容器とを備え、前記蓋部材が前記開口部を開閉自在に前記容器に外嵌及び取り外し可能であって、前記反応室にて前記亜塩素酸塩水溶液と前記酸とを反応させる反応工程において、前記反応器を水浴中に水没させて、フック部材を前記取っ手部材に引っ掛けて、前記蓋部材を前記容器から持ち上げることにより前記容器の外周面と前記蓋部材の内周面との間に前記水浴中に下向きに入り込ませる前記連通路を形成するとともに、前記連通路の端部を前記水浴中に開口させる点にある。 A first characteristic configuration of the present invention includes a reaction chamber capable of generating a chlorine dioxide aqueous solution by reacting a chlorite aqueous solution and an acid, and a communication path capable of communicating between the upper portion of the reaction chamber and the outside of the reaction chamber. A method for producing an aqueous chlorine dioxide solution using a reactor equipped with the reactor, wherein the reactor comprises a lid member having a handle member on the upper surface, a container having the reaction chamber on the inner side and an opening on the upper side, In the reaction step of allowing the lid member to be externally fitted to and removed from the container so that the opening can be opened and closed, and reacting the chlorite aqueous solution and the acid in the reaction chamber , the reaction A vessel is submerged in a water bath, a hook member is hooked on the handle member, and the lid member is lifted from the container, whereby the container is placed between the outer peripheral surface of the container and the inner peripheral surface of the lid member. the communication to enter downwardly To form a, there an end of the communication passage in that is opened in the water bath.

〔作用及び効果〕
反応室において、高濃度の亜塩素酸塩水溶液と高濃度の酸とを反応させることができるので、反応室内に高濃度の二酸化塩水溶液を生成させることができる。そして、反応室にて発生した二酸化塩素ガスは、反応室内の上部と反応室外とを連通可能な連通路を通じて、反応室とは別個の水浴中に誘導されて溶解する。その結果、二酸化塩素ガスの大気中への放出が減少して、悪臭等の環境汚染を防止し得る。しかも、その連通路は水浴中に下向きに入り込ませてあるので、水浴中の水が連通路中に浸入するのを防止できる。よって、水浴中の水は反応室内に浸入せず、生成された二酸化塩素水溶液が希釈されてしまうこともないので、高濃度で生成効率の高い二酸化塩素水溶液が生成され得る。従って、本発明によれば、二酸化塩素ガスによる悪臭等の環境汚染を防止し得ると同時に高濃度で生成効率の高い二酸化塩素水溶液を製造することができる。 [Action and effect]
Since a high concentration chlorite aqueous solution and a high concentration acid can be reacted in the reaction chamber, a high concentration salt dioxide aqueous solution can be generated in the reaction chamber. The chlorine dioxide gas generated in the reaction chamber is guided and dissolved in a water bath separate from the reaction chamber through a communication path that allows communication between the upper portion of the reaction chamber and the outside of the reaction chamber. As a result, the release of chlorine dioxide gas into the atmosphere is reduced, and environmental pollution such as malodor can be prevented. In addition, since the communication path enters downward in the water bath, it is possible to prevent water in the bath from entering the communication path. Therefore, the water in the water bath does not enter the reaction chamber, and the generated chlorine dioxide aqueous solution is not diluted, so that a chlorine dioxide aqueous solution having a high concentration and high production efficiency can be produced. Therefore, according to the present invention, it is possible to produce an aqueous chlorine dioxide solution with high concentration and high production efficiency while preventing environmental pollution such as bad odor due to chlorine dioxide gas.

本発明の第２特徴構成は、前記亜塩素酸塩水溶液の濃度が１０重量％以上２５重量％以下であり、前記酸の濃度が５重量％以上１０重量％未満である点にある。
〔作用及び効果〕
後述するように、高濃度で生成効率の高い二酸化塩素水溶液を効率よく製造することができる。さらに、酸の濃度を１０重量％未満にすることにより、危険物取扱い上の法規の規制を受けることなく、原料の貯蔵、取扱いに特別な資格を必要としないので誰でも簡便に二酸化塩素水溶液を製造することができる。 The second characteristic configuration of the present invention is that the concentration of the chlorite aqueous solution is 10 wt% or more and 25 wt% or less, and the concentration of the acid is 5 wt% or more and less than 10 wt%.
[Action and effect]
As will be described later, a chlorine dioxide aqueous solution having a high concentration and high production efficiency can be efficiently produced. Furthermore, by making the acid concentration less than 10% by weight, no special qualifications are required for storage and handling of raw materials without any restrictions on the handling of dangerous goods, so anyone can easily use an aqueous chlorine dioxide solution. Can be manufactured.

以下に本発明の実施の形態を図面に基づいて説明する。   Embodiments of the present invention will be described below with reference to the drawings.

〔第１参考例〕
図１は、亜塩素酸塩水溶液と酸とを反応させて二酸化塩素水溶液を生成可能な反応室４と、前記反応室４内の上部と反応室４外とを連通可能な連通路６とを備えた反応器１を使用して二酸化塩素水溶液を製造する、本発明の二酸化塩素水溶液製造方法を示している。 [ First Reference Example ]
FIG. 1 shows a reaction chamber 4 capable of producing a chlorine dioxide aqueous solution by reacting a chlorite aqueous solution with an acid, and a communication passage 6 capable of communicating between the upper portion of the reaction chamber 4 and the outside of the reaction chamber 4. The chlorine dioxide aqueous solution manufacturing method of this invention which manufactures chlorine dioxide aqueous solution using the equipped reactor 1 is shown.

つまり、前記反応器１は、周壁８の内周面９に雌ねじが設けられている蓋部材５を、容器３の上部開口２周りの容器外周面１０に設けられた雄ねじにねじ込んだり、あるいは緩めたりすることにより上部開口２を開閉自在な密閉容器を使用して構成してあり、例えば、市販の、キャップを備えた褐色等に着色してあるねじ口瓶等が使用できる。   That is, in the reactor 1, the lid member 5 provided with the female screw on the inner peripheral surface 9 of the peripheral wall 8 is screwed into the male screw provided on the outer peripheral surface 10 around the upper opening 2 of the container 3 or loosened. For example, a commercially available screw-mouth bottle colored in brown or the like with a cap can be used.

そして、前記容器３の内側を、Ａ液（亜塩素酸ナトリウム水溶液）とＢ液（塩酸）とを反応させて二酸化塩素水溶液を生成可能な反応室４に形成するともに、蓋部材５の固定を緩めることにより容器外周面１０と蓋部材５における周壁８の内周面９との間に、反応室４内の上部と反応室外とを連通可能な連通路６が形成される。   And the inside of the said container 3 is formed in the reaction chamber 4 which can produce | generate chlorine dioxide aqueous solution by making A liquid (sodium chlorite aqueous solution) and B liquid (hydrochloric acid) react, and fixing of the cover member 5 is carried out. By loosening, a communication path 6 is formed between the container outer peripheral surface 10 and the inner peripheral surface 9 of the peripheral wall 8 of the lid member 5 so that the upper part in the reaction chamber 4 can communicate with the outside of the reaction chamber.

製造工程としては、まず、図１（イ）に示すように、Ａ液及びＢ液を夫々容器３に入れて、図１（ロ）に示すように蓋部材５をねじ込み固定し、容器３を数回振って、上記薬液を混合する（混合工程）。   As a manufacturing process, first, as shown in FIG. 1 (a), the A liquid and the B liquid are respectively put into the container 3, and the lid member 5 is screwed and fixed as shown in FIG. Shake several times to mix the chemical solution (mixing step).

次いで、図１（ハ）に示すように蓋部材５のねじ込み固定を緩めて連通路６を設け、そして、容器３全体を、反応室４とは別個の、例えばポリバケツ等の水槽７に設けた水浴（ウォーターバス）１６中に沈め、連通路６の端部を水浴１６中で下向きに開口させ、そのまま一定時間（好ましくは、１０〜２０分程度）放置し、反応室４にてＡ液とＢ液とを反応させて、容器３の中に二酸化塩素水溶液を生成する（反応工程）。   Next, as shown in FIG. 1 (c), the screwing and fixing of the lid member 5 is loosened to provide a communication passage 6, and the entire container 3 is provided in a water tank 7 such as a poly bucket separate from the reaction chamber 4. Submerged in a water bath (water bath) 16, the end of the communication path 6 is opened downward in the water bath 16, and left as it is for a certain period of time (preferably about 10 to 20 minutes). The B liquid is reacted to produce an aqueous chlorine dioxide solution in the container 3 (reaction process).

〔第２参考例〕
図２は、本発明の二酸化塩素水溶液製造方法の第２参考例を示し、反応器１は、上部に開口部２を設けてある容器３（例えば、市販の、褐色等に着色してある試薬瓶等）の開口部２に、反応室４内の上部と反応室外とを連通する貫通孔１１が設けられている蓋部材５（例えばゴム栓等）を押し込んで内嵌させ、そしてさらにその貫通孔１１（貫通孔１１の内径の大きさは、中空管１２の外径の大きさと同じか、もしくはそれよりも小さく形成されている）内に中空管１２（例えば、ゴム管、樹脂管、ガラス管等）の先端を挿し込んで接続して構成してある。 [ Second Reference Example ]
FIG. 2 shows a second reference example of the method for producing a chlorine dioxide aqueous solution of the present invention. The reactor 1 has a container 3 (for example, a commercially available reagent colored brown or the like) provided with an opening 2 in the upper part. A lid member 5 (for example, a rubber plug) provided with a through hole 11 that communicates the upper part in the reaction chamber 4 with the outside of the reaction chamber is pushed into the opening 2 of the bottle or the like, and is further fitted inside. The hollow tube 12 (for example, rubber tube, resin tube) is formed in the hole 11 (the inner diameter of the through-hole 11 is the same as or smaller than the outer diameter of the hollow tube 12). The tip of a glass tube or the like is inserted and connected.

そして、容器３の内側を、Ａ液（亜塩素酸ナトリウム水溶液）とＢ液（塩酸）とを反応させて二酸化塩素水溶液を生成可能な反応室４に形成するともに、蓋部材５および中空管１２を開口部２に接続することにより、反応室４内の上部と反応室外とを連通可能な連通路６が形成される。   And the inside of the container 3 is formed in the reaction chamber 4 in which the liquid A (sodium chlorite aqueous solution) and the liquid B (hydrochloric acid) are reacted to generate an aqueous chlorine dioxide solution, and the lid member 5 and the hollow tube By connecting 12 to the opening 2, a communication path 6 is formed which allows communication between the upper part in the reaction chamber 4 and the outside of the reaction chamber.

製造工程としては、まず、Ａ液及びＢ液を夫々容器３に入れて混合する（混合工程）。   As a manufacturing process, first, the A liquid and the B liquid are respectively put in the container 3 and mixed (mixing process).

次いで、蓋部材５および中空管１２を開口部２に接続することにより連通路６を設け、連通路６（中空管１２）を反応室４とは別個の、例えばポリバケツ等の水槽７に設けた水浴１６中に下向きに入り込ませるとともに、連通路６の端部を水浴１６中に開口させて、そのまま一定時間（好ましくは、１０〜２０分程度）放置し、反応室４にてＡ液とＢ液とを反応させて容器３の中に二酸化塩素水溶液を生成する（反応工程）。   Next, the communication channel 6 is provided by connecting the lid member 5 and the hollow tube 12 to the opening 2, and the communication channel 6 (hollow tube 12) is separated from the reaction chamber 4 in a water tank 7 such as a poly bucket. Into the water bath 16 provided, the end of the communication path 6 is opened in the water bath 16 and left as it is for a certain time (preferably about 10 to 20 minutes). And B solution are reacted to produce an aqueous chlorine dioxide solution in the container 3 (reaction process).

〔第３参考例〕
図３は、本発明の二酸化塩素水溶液製造方法の第３参考例を示し、反応器１は、上部に開口部２を設けてある容器３（例えば、市販の、褐色等に着色してある試薬瓶など）の開口部２に、反応室４内の上部と反応室外とを連通する貫通孔１１が設けられている蓋部材５（例えばゴム栓等）を押し込んで内嵌させ、そしてさらにその貫通孔１１を、気体の通過は許容し液体の通過は阻止するという選択性透過部材１３（例えば、気液分離フィルタ等の分離膜部材）で塞いで構成してある。 [ Third reference example ]
FIG. 3 shows a third reference example of the method for producing an aqueous chlorine dioxide solution of the present invention, in which the reactor 1 is a container 3 (for example, a commercially available reagent colored brown or the like) provided with an opening 2 in the upper part. A lid member 5 (for example, a rubber plug) provided with a through hole 11 that communicates the upper part in the reaction chamber 4 with the outside of the reaction chamber is pushed into the opening 2 of the bottle or the like, and is further fitted inside. The hole 11 is configured by being closed with a selective transmission member 13 (for example, a separation membrane member such as a gas-liquid separation filter) that allows passage of gas and blocks passage of liquid.

そして、容器３の内側を、Ａ液（亜塩素酸ナトリウム水溶液）とＢ液（塩酸）とを反応させて二酸化塩素水溶液を生成可能な反応室４に形成するともに、上記選択性透過部材１３で貫通孔１１を塞いである蓋部材５を上部開口２に接続することにより、反応室４内の上部と反応室外とを気体のみが連通可能な連通路６が形成される。   Then, the inside of the container 3 is formed in the reaction chamber 4 capable of generating a chlorine dioxide aqueous solution by reacting the liquid A (sodium chlorite aqueous solution) and the liquid B (hydrochloric acid). By connecting the lid member 5 that closes the through-hole 11 to the upper opening 2, a communication path 6 is formed that allows only gas to communicate between the upper part in the reaction chamber 4 and the outside of the reaction chamber.

製造工程としては、まず、Ａ液及びＢ液を夫々容器３に入れて混合する（混合工程）。   As a manufacturing process, first, the A liquid and the B liquid are respectively put in the container 3 and mixed (mixing process).

次いで、上記蓋部材５を上部開口２に接続することにより上記連通路６を設け、容器３全体を、反応室４とは別個の、例えばポリバケツ等の水槽７に設けた水浴１６中に沈めて、連通路６の端部を水浴１６中に開口させて、そのまま一定時間（好ましくは、１０〜２０分程度）放置し、反応室４にてＡ液とＢ液とを反応させて、容器３の中に二酸化塩素水溶液を生成する（反応工程）。   Next, by connecting the lid member 5 to the upper opening 2, the communication path 6 is provided, and the entire container 3 is submerged in a water bath 16 provided in a water tank 7 such as a poly bucket separate from the reaction chamber 4. The end of the communication path 6 is opened in the water bath 16 and left as it is for a certain period of time (preferably about 10 to 20 minutes), and the A liquid and the B liquid are reacted in the reaction chamber 4, and the container 3 A chlorine dioxide aqueous solution is produced in the reaction chamber (reaction process).

〔実施形態〕
図４は、本発明の二酸化塩素水溶液製造方法の実施形態を示し、反応器１は、上面にＵ字型の取っ手部材１４を備える蓋部材５を、容器３の上部開口２周りの容器外周面に外嵌したり、あるいは外したりすることにより上部開口２を開閉自在な密閉容器を使用して構成してある。 [Implementation Embodiment
Figure 4 shows an implementation form of the aqueous solution of chlorine dioxide production method of the present invention, the reactor 1, the lid member 5 comprises a handle member 14 of the U-shaped on the upper surface, the container periphery around the upper opening 2 of the container 3 The upper opening 2 is configured by using a sealed container that can be freely opened and closed by being externally fitted to or removed from the surface.

そして、容器３の内側を、Ａ液（亜塩素酸ナトリウム水溶液）とＢ液（塩酸）とを反応させて二酸化塩素水溶液を生成可能な反応室４に形成するともに、Ｕ字型の取っ手部材１４に引っ掛け可能なフック部材１５を前記取っ手部材１４に引っ掛けて、蓋部材５を容器３から外れない程度に少しだけ持ち上げることにより、反応室４内の上部と反応室外とを連通可能な連通路６が形成される。   The inside of the container 3 is formed in the reaction chamber 4 capable of producing a chlorine dioxide aqueous solution by reacting the liquid A (sodium chlorite aqueous solution) and the liquid B (hydrochloric acid), and a U-shaped handle member 14. The hook member 15 that can be hooked on the handle member 14 is hooked on the handle member 14 and the lid member 5 is slightly lifted to the extent that it cannot be removed from the container 3. Is formed.

製造工程としては、まず、Ａ液及びＢ液を夫々容器３に入れて混合し、蓋部材５を外嵌する（混合工程）。   As a manufacturing process, first, the A liquid and the B liquid are respectively put in the container 3 and mixed, and the lid member 5 is externally fitted (mixing process).

次いで、容器３全体を、反応室４とは別個の、例えばポリバケツ等の水槽７に設けた水浴１６中に沈めて、フック部材１５をＵ字型の取っ手部材１４に引っ掛け、蓋部材５を容器３から外れない程度に少しだけ持ち上げることにより連通路６を設け、連通路６の端部を水浴１６中に下向きに開口させて、そのまま一定時間（好ましくは、１０〜２０分程度）放置し、反応室４にてＡ液とＢ液とを反応させて、容器３の中に二酸化塩素水溶液を生成する（反応工程）。   Next, the entire container 3 is submerged in a water bath 16 provided in a water tank 7 such as a poly bucket separate from the reaction chamber 4, and the hook member 15 is hooked on the U-shaped handle member 14, and the lid member 5 is placed in the container. The communication path 6 is provided by slightly lifting it up so that it does not deviate from 3, and the end of the communication path 6 is opened downward in the water bath 16 and left as it is for a certain time (preferably about 10 to 20 minutes). The liquid A and the liquid B are reacted in the reaction chamber 4 to generate an aqueous chlorine dioxide solution in the container 3 (reaction process).

〔その他の実施形態〕
１．本発明による二酸化塩素水溶液製造方法は、Ａ液の亜塩素酸塩水溶液として、亜塩素酸カリウム、亜塩素酸カルシウム等の亜塩素酸のアルカリ金属塩あるいはアルカリ土類金属塩の水溶液を使用するものであっても良い。
２．本発明による二酸化塩素水溶液製造方法は、Ｂ液の酸として、硫酸、リン酸などの鉱酸やクエン酸、酒石酸等の有機酸を使用するものであっても良い。
３．本発明による二酸化塩素水溶液製造方法は、１個の水浴に対して、複数の反応器を使用するような構成であっても良い。
４．本発明による二酸化塩素水溶液製造方法において、反応器と水浴中とに同時に所望の濃度の二酸化塩素水溶液が製造され得る構成であっても良い。 [Other Embodiments]
1. The method for producing an aqueous chlorine dioxide solution according to the present invention uses an aqueous solution of an alkali metal salt or alkaline earth metal salt of chlorite such as potassium chlorite and calcium chlorite as the chlorite solution of solution A. It may be.
2. The chlorine dioxide aqueous solution production method according to the present invention may use a mineral acid such as sulfuric acid or phosphoric acid or an organic acid such as citric acid or tartaric acid as the acid for the B solution.
3. The chlorine dioxide aqueous solution production method according to the present invention may be configured to use a plurality of reactors for one water bath.
4). The chlorine dioxide aqueous solution production method according to the present invention may be configured such that a chlorine dioxide aqueous solution having a desired concentration can be produced simultaneously in the reactor and the water bath.

上記第１参考例について、Ａ液として１０重量％以上２５重量％以下の亜塩素酸ナトリウム水溶液及び、Ｂ液として５重量％以上１０重量％未満の塩酸水溶液を使用し、水浴温度と二酸化塩素ガス濃度を種々に変えて二酸化塩素水溶液を生成した結果を図５に示す。 About the said 1st reference example , 10 to 25 weight% of sodium chlorite aqueous solution is used as A liquid, and 5 to 10 weight% of hydrochloric acid aqueous solution is used as B liquid, water bath temperature and chlorine dioxide gas FIG. 5 shows the result of producing a chlorine dioxide aqueous solution with various concentrations.

図５によると、２０℃ １ａｔｍにおける二酸化塩素の溶解度はおよそ９０ｇ／Ｌであり、この結果から、本発明の二酸化塩素水溶液製造方法は、常温常圧において、およそ１０3〜１０5ｐｐｍの二酸化塩素水溶液を製造し得るものと推察された。 According to FIG. 5, the solubility of chlorine dioxide at 20 ° C. and 1 atm is approximately 90 g / L. From this result, the chlorine dioxide aqueous solution production method of the present invention is approximately 10 3 to 10 5 ppm of chlorine dioxide at room temperature and normal pressure. It was speculated that an aqueous solution could be produced.

また、図６に示されるように、実施例１〜９として、８〜２５重量％の亜塩素酸ナトリウム水溶液と、９重量％の塩酸とを反応させて、二酸化塩素水溶液を生成し、反応器および水浴中の二酸化塩素濃度を測定し、生成効率を算出した。   Moreover, as shown in FIG. 6, as Examples 1-9, 8-25 weight% sodium chlorite aqueous solution and 9 weight% hydrochloric acid were made to react, a chlorine dioxide aqueous solution was produced | generated, and a reactor The chlorine dioxide concentration in the water bath was measured, and the production efficiency was calculated.

尚、比較例１〜４として、０．２５〜０.５重量％の亜塩素酸ナトリウム水溶液と、０.４重量％のシュウ酸（比較例１）又は９重量％の塩酸とを反応させて、同様の試験を行った。   As Comparative Examples 1 to 4, 0.25 to 0.5% by weight of sodium chlorite aqueous solution was reacted with 0.4% by weight of oxalic acid (Comparative Example 1) or 9% by weight of hydrochloric acid. A similar test was conducted.

〔化１〕
５ＣｌＯ2 -＋４Ｈ+→４ＣｌＯ2＋２Ｈ2Ｏ＋Ｃｌ- [Chemical formula 1]
5ClO 2 − + 4H + → 4ClO 2 + 2H 2 O + Cl −

図６における、酸過剰率（％）とは、亜塩素酸塩と反応する酸の理論量に対して実際に使用した酸の量を示し、亜塩素酸塩と酸から二酸化塩素が生成される上記反応式に示されるように、５ｍｏｌの亜塩素酸塩に対して４ｍｏｌの水素イオン（塩酸なら４ｍｏｌ、シュウ酸なら２ｍｏｌ）を使用した場合を１００％とした値である。   In FIG. 6, the acid excess (%) indicates the amount of acid actually used with respect to the theoretical amount of acid that reacts with chlorite, and chlorine dioxide is generated from the chlorite and acid. As shown in the above reaction formula, this value is 100% when 4 mol of hydrogen ions (4 mol for hydrochloric acid and 2 mol for oxalic acid) are used per 5 mol of chlorite.

また、生成効率（％）とは、使用された亜塩素酸塩から生成され得る二酸化塩素の理論量に対して実際に発生した二酸化塩素の発生率を示し、上記反応式１に示されるように、５ｍｏｌの亜塩素酸塩に対して４ｍｏｌの二酸化塩素が生成された場合を１００％とした値である。   The production efficiency (%) indicates the generation rate of chlorine dioxide actually generated with respect to the theoretical amount of chlorine dioxide that can be generated from the used chlorite, and as shown in the above reaction formula 1. The value is 100% when 4 mol of chlorine dioxide is produced with respect to 5 mol of chlorite.

図６によれば、実施例１〜９における生成効率は５５％〜６２％であり、比較例１〜４における１１％〜３５％と比べて、生成効率がかなり高くなることが判明した。   According to FIG. 6, the production efficiencies in Examples 1 to 9 are 55% to 62%, and the production efficiencies are considerably higher than those in Comparative Examples 1 to 4 of 11% to 35%.

第１参考例の二酸化塩素水溶液製造方法を示す概略図Schematic showing the chlorine dioxide aqueous solution manufacturing method of the first reference example 第２参考例の二酸化塩素水溶液製造方法を示す概略図Schematic showing the chlorine dioxide aqueous solution manufacturing method of the second reference example 第３参考例の二酸化塩素水溶液製造方法を示す概略図Schematic showing the chlorine dioxide aqueous solution manufacturing method of the third reference example 実施形態の二酸化塩素水溶液製造方法を示す概略図Schematic which shows the chlorine dioxide aqueous solution manufacturing method of embodiment 第１参考例の二酸化塩素水溶液製造方法により得られた、二酸化塩素ガスの水１リットルに対する溶解度を示す図 The figure which shows the solubility with respect to 1 liter of water of the chlorine dioxide gas obtained by the chlorine dioxide aqueous solution manufacturing method of the 1st reference example 第１参考例の二酸化塩素水溶液製造方法により得られた、二酸化塩素ガスの生成効率等を示す図表Chart showing the production efficiency of chlorine dioxide gas obtained by the chlorine dioxide aqueous solution manufacturing method of the first reference example

１ 反応器
２ 開口部
３ 容器
４ 反応室
５ 蓋部材
６ 連通路
７ 水槽
９ 周壁内周面
１０ 容器外周面
１２ 中空管
１３ 選択性透過部材
１６ 水浴 DESCRIPTION OF SYMBOLS 1 Reactor 2 Opening part 3 Container 4 Reaction chamber 5 Lid member 6 Communication path 7 Water tank 9 Perimeter wall inner peripheral surface 10 Container outer peripheral surface 12 Hollow pipe 13 Selective permeation member 16 Water bath

Claims (2)

亜塩素酸塩水溶液と酸とを反応させて二酸化塩素水溶液を生成可能な反応室と、前記反応室内の上部と前記反応室外とを連通可能な連通路とを備えた反応器を使用して二酸化塩素水溶液を製造する方法であって、
前記反応器が、上面に取っ手部材を備える蓋部材と、内側に前記反応室を有し上部に開口部を有する容器とを備え、前記蓋部材が前記開口部を開閉自在に前記容器に外嵌及び取り外し可能であって、
前記反応室にて前記亜塩素酸塩水溶液と前記酸とを反応させる反応工程において、前記反応器を水浴中に水没させて、フック部材を前記取っ手部材に引っ掛けて、前記蓋部材を前記容器から持ち上げることにより前記容器の外周面と前記蓋部材の内周面との間に前記水浴中に下向きに入り込ませる前記連通路を形成するとともに、前記連通路の端部を前記水浴中に開口させる二酸化塩素水溶液製造方法。 Using a reactor equipped with a reaction chamber capable of reacting a chlorite aqueous solution with an acid to produce a chlorine dioxide aqueous solution, and a communication passage capable of communicating the upper part of the reaction chamber and the outside of the reaction chamber, A method for producing a chlorine aqueous solution,
The reactor includes a lid member having a handle member on an upper surface thereof, and a container having the reaction chamber on the inner side and an opening portion on the upper side, and the lid member is externally fitted to the container so that the opening portion can be opened and closed. And removable,
In the reaction step of reacting the chlorite aqueous solution and the acid in the reaction chamber , the reactor is submerged in a water bath, a hook member is hooked on the handle member, and the lid member is removed from the container. The communication passage is formed between the outer peripheral surface of the container and the inner peripheral surface of the lid member by being lifted so as to enter the water bath downward, and the end portion of the communication passage is opened in the water bath. Chlorine aqueous solution manufacturing method. 前記亜塩素酸塩水溶液の濃度が１０重量％以上２５重量％以下であり、前記酸の濃度が５重量％以上１０重量％未満である、請求項１に記載の二酸化塩素水溶液製造方法。   The method for producing a chlorine dioxide aqueous solution according to claim 1, wherein the concentration of the chlorite aqueous solution is 10 wt% or more and 25 wt% or less, and the concentration of the acid is 5 wt% or more and less than 10 wt%.
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