JP4862191B2 - Method for treating selenium-containing water - Google Patents
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Description
本発明は、セレン含有水の処理方法に関し、特に、製錬工程やセレンの製造・加工工程から排出されたセレン含有排水などのセレン含有水を処理する方法に関する。 The present invention relates to a method for treating selenium-containing water, and more particularly, to a method for treating selenium-containing water such as selenium-containing wastewater discharged from a smelting process or a selenium production / processing process.
従来、セレン含有水の処理方法として、鉄粉置換処理法、２価鉄を用いた還元処理法、３価鉄を用いた共沈法などが知られているが、平成５年８月の水質汚濁防止法施行令の一部改正によりセレンに関する排水基準が０．１ｍｇ／Ｌ以下と規定されたことに伴い、セレンの除去能力の高い処理技術の開発が進められてきた。 Conventionally, as a method for treating selenium-containing water, there are known an iron powder replacement treatment method, a reduction treatment method using divalent iron, a coprecipitation method using trivalent iron, and the like. With the revision of the Ordinance on Enforcement of the Pollution Control Act, the selenium drainage standard was stipulated to be 0.1 mg / L or less, and the development of treatment technology with high selenium removal capability has been promoted.
近年、セレンの除去能力の高い方法として、セレン含有排水に弱酸性下で２価鉄イオンを添加し、さらに還元剤を用いて液の酸化還元電位を極低電位レベルまで低下させ、次いで急速に中和処理して２価鉄イオンを水酸化鉄として晶出させ、中和処理した後、固液分離することによりセレンを除去する方法が提案されている（例えば、特許文献１参照）。また、その他の方法として、セレンと反応して難溶性塩を生成する金属塩をセレン含有水に添加する方法、セレン含有水を生物汚泥と嫌気状態で接触させてセレン化合物を沈殿除去する方法、Ｆｅなどの金属を排煙脱硫排水に接触させて排煙脱硫排水中の酸化性物質とセレンを除去する方法、イオン交換樹脂またはキレート樹脂にセレンを吸着させる方法、セレン含有液に銅塩を添加した後にアルカリを添加して凝集物を分離することによりセレンを除去する方法、６価セレン含有排水を遷移金属化合物と還元剤との存在下でセレンを沈殿として除去する方法などが提案されている（例えば、特許文献２〜７参照）。
In recent years, as a method having a high ability to remove selenium, divalent iron ions are added to selenium-containing wastewater under weak acidity, and the redox potential of the liquid is lowered to a very low potential level using a reducing agent, and then rapidly. There has been proposed a method of removing selenium by performing neutralization treatment to crystallize divalent iron ions as iron hydroxide, neutralization treatment, and solid-liquid separation (see, for example, Patent Document 1). In addition, as another method, a method of adding a metal salt that reacts with selenium to form a hardly soluble salt to selenium-containing water, a method of bringing selenium-containing water into contact with biological sludge in an anaerobic state, and precipitating and removing selenium compounds, A method of removing metal and selenium from the flue gas desulfurization waste water by contacting a metal such as Fe with the flue gas desulfurization waste water, a method of adsorbing selenium to an ion exchange resin or a chelate resin, and adding a copper salt to the selenium-containing liquid After that, a method for removing selenium by adding an alkali to separate aggregates and a method for removing selenium as a precipitate from a hexavalent selenium-containing wastewater in the presence of a transition metal compound and a reducing agent have been proposed. (For example, refer to
このように、排水中のセレンを安全に分離し且つ厳しい排出規制に沿って無害化する様々な方法が提案されている。しかし、これらの方法には、セレン以外の多くの沈殿物が残留したり、対象排水の制限により所望のセレンの除去率を得ることができない場合にセレンの回収効率を高めるために過剰な設備が必要であったり、使用する試薬が高価であったり、プロセスが煩雑であったりするなどの問題がある。また、回収したセレンを非鉄金属製錬の原料として使用可能な状態に分離できないという問題もある。 As described above, various methods for safely separating selenium in waste water and detoxifying it in accordance with strict emission regulations have been proposed. However, these methods have excessive facilities to increase the recovery efficiency of selenium when a large amount of precipitate other than selenium remains or the desired selenium removal rate cannot be obtained due to restrictions on the target wastewater. There are problems such as necessity, expensive reagents used, and complicated processes. There is also a problem that the recovered selenium cannot be separated into a usable state as a raw material for non-ferrous metal smelting.
したがって、本発明は、このような従来の問題点に鑑み、セレン含有水から高い除去率で簡単且つ安価にセレンを除去することができるとともに、セレン含有水からセレンを含む化合物を効率的に分離して回収することができる、セレン含有水の処理方法を提供することを目的とする。 Therefore, in view of such conventional problems, the present invention can easily and inexpensively remove selenium from selenium-containing water at a high removal rate, and efficiently separate selenium-containing compounds from selenium-containing water. It is an object of the present invention to provide a method for treating selenium-containing water that can be recovered in the same manner.
本発明者らは、上記課題を解決するために鋭意研究した結果、セレン含有水に銅またはその化合物を添加した後、銅よりもイオン化傾向が大きい金属の粉末を添加して沈殿物を生成させることにより、セレン含有水から高い除去率で簡単且つ安価にセレンを除去することができるとともに、セレン含有水からセレンを含む化合物を効率的に分離して回収することができることを見出し、本発明を完成するに至った。 As a result of diligent research to solve the above problems, the present inventors have added copper or a compound thereof to selenium-containing water, and then added a metal powder having a higher ionization tendency than copper to generate a precipitate. Thus, it has been found that selenium can be easily and inexpensively removed from selenium-containing water at a high removal rate and that selenium-containing compounds can be efficiently separated and recovered from selenium-containing water. It came to be completed.
すなわち、本発明によるセレン含有水の処理方法は、セレン含有水に銅またはその化合物を添加した後、銅よりもイオン化傾向が大きい金属の粉末を添加して沈殿物を生成させることを特徴とする。このセレン含有水の処理方法において、銅（Ｃｕ）よりもイオン化傾向が大きい金属が、アルミニウム（Ａｌ）、亜鉛（Ｚｎ）、鉄（Ｆｅ）、ニッケル（Ｎｉ）、コバルト（Ｃｏ）、錫（Ｓｎ）および鉛（Ｐｂ）からなる群から選ばれる金属であるのが好ましい。また、セレン含有水に添加する銅の量が、セレン含有水中のセレン（Ｓｅ）１重量部に対して０．５〜１．５重量部であるのが好ましく、０．７〜１．２重量部であるのがさらに好ましい。また、銅またはその化合物が、銅の粉末またはその硫酸塩、硝酸塩または塩化物、あるいは、製錬工程で使用される電解液であるのが好ましい。また、銅よりもイオン化傾向が大きい金属の粉末を添加する際に、酸化還元電位（Ａｇ／ＡｇＣｌ電極（銀／塩化銀電極））を＋５０〜−４００ｍＶにするのが好ましく、−１００〜−３００ｍＶにするのがさらに好ましい。さらに、セレン含有水中のＳｅ濃度が５ｍｇ／Ｌ以上であるのが好ましい。 That is, the method for treating selenium-containing water according to the present invention is characterized in that after adding copper or a compound thereof to selenium-containing water, a metal powder having a higher ionization tendency than copper is added to generate a precipitate. . In this selenium-containing water treatment method, metals having a higher ionization tendency than copper (Cu) are aluminum (Al), zinc (Zn), iron (Fe), nickel (Ni), cobalt (Co), tin (Sn). And a metal selected from the group consisting of lead (Pb). Moreover, it is preferable that the quantity of the copper added to selenium containing water is 0.5 to 1.5 weight part with respect to 1 weight part of selenium (Se) in selenium containing water, and 0.7 to 1.2 weight. More preferably, it is part. Further, copper or a compound thereof is preferably copper powder or a sulfate, nitrate or chloride thereof, or an electrolytic solution used in a smelting process. Further, when adding a metal powder having a higher ionization tendency than copper, the oxidation-reduction potential (Ag / AgCl electrode (silver / silver chloride electrode)) is preferably +50 to −400 mV, and −100 to −300 mV. More preferably. Furthermore, the Se concentration in the selenium-containing water is preferably 5 mg / L or more.
なお、本明細書中において、「金属の粉末」とは、粒径が数μｍ〜数ｍｍの金属の粒状物をいい、粒径が数μｍの金属の粉末が担持体に担持された場合も含まれ、金属の粉末がセレン含有水に接触することができる形態であればよい。 In the present specification, “metal powder” refers to metal particles having a particle size of several μm to several mm, and a metal powder having a particle size of several μm may be supported on a carrier. Any form that is included and can contact the selenium-containing water is acceptable.
本発明によれば、セレン含有水から高い除去率で簡単且つ安価にセレンを除去することができるとともに、セレン含有水からセレンを含む化合物を効率的に分離して回収することができる。 According to the present invention, selenium can be easily and inexpensively removed from selenium-containing water at a high removal rate, and a compound containing selenium can be efficiently separated and recovered from selenium-containing water.
以下、添付図面を参照して、本発明によるセレン含有水の処理方法の実施の形態について説明する。 Hereinafter, with reference to an accompanying drawing, an embodiment of a processing method of selenium content water by the present invention is described.
図１は、本発明によるセレン含有水の処理方法の一実施の形態を説明する工程図である。図１に示すように、まず、処理対象であるセレン含有水として、製錬工程から排出されたセレン含有排水を用意する。このセレン含有排水は、Ｓｅイオンとして、例えば９０％程度の４価のＳｅイオンと１０％程度の６価のＳｅイオンを含んでいる。 FIG. 1 is a process diagram illustrating one embodiment of a method for treating selenium-containing water according to the present invention. As shown in FIG. 1, first, selenium-containing wastewater discharged from the smelting process is prepared as selenium-containing water to be treated. This selenium-containing wastewater contains, for example, about 90% of tetravalent Se ions and about 10% of hexavalent Se ions as Se ions.
次に、セレン含有排水にＣｕ粉または硫酸銅（ＣｕＳＯ４）を添加する。Ｃｕ粉を添加すると、セレンが還元されてセレン含有排水中のＳｅ濃度が約５０％になる。一方、ＣｕＳＯ４を添加しても、セレン含有排水中のＳｅ濃度は変化しない。なお、ここで添加するＣｕ粉の量は、セレン含有水中のセレン１重量部に対して０．５〜１．５重量部であるのが好ましく、０．７〜１．２重量部であるのがさらに好ましい。 Next, Cu powder or copper sulfate (CuSO 4 ) is added to the selenium-containing waste water. When Cu powder is added, selenium is reduced and the Se concentration in the selenium-containing wastewater becomes about 50%. On the other hand, even if CuSO 4 is added, the Se concentration in the selenium-containing wastewater does not change. In addition, it is preferable that the quantity of Cu powder added here is 0.5-1.5 weight part with respect to 1 weight part of selenium in selenium containing water, and is 0.7-1.2 weight part. Is more preferable.
次に、セレン含有排水にＦｅ粉やＺｎ粉などの銅よりもイオン化傾向が大きい金属の粉末を添加すると、セメンテーションによって還元電位が下がって置換反応が起こり、沈殿物が生成する。このセメンテーションを生じさせるために添加する金属粉末の量は、添加したＣｕ粉の量によって決定され、Ｃｕに対して１モル当量以上であることが必要であり、電位の制御を考慮すると、１．１モル当量以上であるのが好ましい。但し、２．０モル当量以上であると、電位を必要以上に下げて、金属粉末の添加量の増大に伴うコストアップにつながるとともに、析出したＣｕの純度を低下する（セメンテーション用の金属粉末の溶け残りがコンタミネーションになる）ので、好ましくない。したがって、金属粉末の添加量は、Ｃｕに対して１．０〜２．０モル当量であるのが好ましく、１．１〜１．５モル当量であるのがさらに好ましい。この金属の粉末を添加する際に、酸化還元電位（Ａｇ／ＡｇＣｌ電極）を＋５０〜−４００ｍＶにするのが好ましく、−１００〜−３００ｍＶにするのがさらに好ましい。なお、このときの液温は、０℃以上で１００℃未満であればよく、１０〜６０℃であるのが好ましく、特別に加温することなく室温でもよい。 Next, when a metal powder having a higher ionization tendency than copper, such as Fe powder or Zn powder, is added to the selenium-containing wastewater, the reduction potential is lowered by cementation, causing a substitution reaction, and a precipitate is generated. The amount of metal powder added to cause this cementation is determined by the amount of added Cu powder and needs to be 1 molar equivalent or more with respect to Cu. .1 molar equivalent or more is preferred. However, if it is 2.0 molar equivalents or more, the potential is lowered more than necessary, leading to an increase in cost associated with an increase in the amount of metal powder added, and the purity of precipitated Cu is reduced (metal powder for cementation). This is not preferable because the undissolved residue is contaminated). Therefore, it is preferable that the addition amount of a metal powder is 1.0-2.0 molar equivalent with respect to Cu, and it is further more preferable that it is 1.1-1.5 molar equivalent. When this metal powder is added, the oxidation-reduction potential (Ag / AgCl electrode) is preferably +50 to −400 mV, more preferably −100 to −300 mV. In addition, the liquid temperature at this time should just be 0 degreeC or more and less than 100 degreeC, it is preferable that it is 10-60 degreeC, and room temperature may be sufficient without heating especially.
このように、Ｃｕ粉またはＣｕＳＯ４を添加したセレン含有排水から脱銅するために、銅よりもイオン化傾向が大きい金属の粉末を添加してセメンテーションによって電位を制御して下げることによって、銅とセレンを同時に除去することができる。このようなセメンテーションを生じさせる金属として、非鉄製錬の場合には、鉄粉や亜鉛を使用するのが好ましい。鉄粉や亜鉛粉を使用すれば、セレン含有水を処理した後に残渣となっても、他の工程で使用することができ、あるいは、その後の処理において特段の設備などが不要であり、コスト面で有利である。なお、銅よりもイオン化傾向が大きい金属であれば、置換反応により脱銅することができる。 Thus, in order to remove copper from selenium-containing wastewater to which Cu powder or CuSO 4 is added, a metal powder having a higher ionization tendency than copper is added and the potential is controlled and lowered by cementation. Selenium can be removed simultaneously. In the case of non-ferrous smelting, it is preferable to use iron powder or zinc as the metal that causes such cementation. If iron powder or zinc powder is used, even if it becomes a residue after treating the selenium-containing water, it can be used in other processes, or no special equipment is required for the subsequent treatment, which is costly. Is advantageous. In addition, if it is a metal with a larger ionization tendency than copper, it can remove copper by a substitution reaction.
次に、上記の金属の添加後に固液分離する。生成した沈殿物は、ＣｕおよびＳｅを含む澱物であり、製錬原料として使用することができる。 Next, solid-liquid separation is performed after the addition of the above metal. The produced | generated deposit is a starch containing Cu and Se, and can be used as a smelting raw material.
次に、液中に塩化バリウム（ＢａＣｌ２）などのバリウム（Ｂａ）塩を添加して、難溶性のＢａ塩を生成することにより、Ｓｅを沈殿させて除去することができる。過剰に投入したＢａＣｌ２は、液のｐＨを中性に戻すために硫酸（Ｈ２ＳＯ４）や硫酸ナトリウム（Ｎａ２ＳＯ４）を添加することよって、ＢａＳＯ４塩として除去することができる。沈殿物は、スラグ原料として自溶炉に戻すことができる。このように、セメンテーション工程で生成する沈殿物と共に固液分離することにより、自溶炉に投入する原料が分離される。 Next, Se can be precipitated and removed by adding a barium (Ba) salt such as barium chloride (BaCl 2 ) to the solution to form a hardly soluble Ba salt. The excessively charged BaCl 2 can be removed as a BaSO 4 salt by adding sulfuric acid (H 2 SO 4 ) or sodium sulfate (Na 2 SO 4 ) in order to return the pH of the solution to neutrality. The precipitate can be returned to the flash furnace as a slag raw material. Thus, the raw material thrown into a flash furnace is isolate | separated by carrying out solid-liquid separation with the precipitate produced | generated by a cementation process.
なお、Ｂａイオンの添加量は、Ｓｅ濃度とＳＯ４濃度によって決定される。これらのイオン濃度が不明である場合には、電気伝導度を測定することにより、過剰なＢａイオンの添加量を最小限にすることができる。例えば、ＢａＣｌ２を添加する場合には、最初にＢａ塩が沈殿するため、電気伝導度が大きく上昇することはないが、過剰のＢａＣｌ２が添加されるとＢａ２＋イオンとＣｌ−イオンのために電気伝導度が上昇する。 The addition amount of Ba ions is determined by the Se concentration and the SO 4 concentration. When the concentration of these ions is unknown, the amount of excess Ba ions added can be minimized by measuring the electrical conductivity. For example, when BaCl 2 is added, since the Ba salt is precipitated first, the electrical conductivity does not increase greatly. However, when excess BaCl 2 is added, it is due to Ba 2+ ions and Cl − ions. The electrical conductivity increases.
以下、本発明によるセレン含有水の処理方法の実施例について詳細に説明する。 Hereinafter, the Example of the processing method of selenium containing water by this invention is described in detail.
［実施例１］
まず、表１に示すように、Ｓｅ１６１．７ｍｇ／Ｌ、Ｃｕ０．５ｍｇ／Ｌ、Ｐｂ１．２１ｍｇ／Ｌ、Ｚｎ４．３ｍｇ／Ｌ、Ｆｅ２．４９ｍｇ／Ｌ、Ａｓ（砒素）６８２．３ｍｇ／Ｌ、Ｈｇ（水銀）１．６μｇ／Ｌを含み、ｐＨ−０．０１、酸化還元電位（ＯＲＰ）（Ａｇ／ＡｇＣｌ電極）３７０ｍＶのセレン含有排水１Ｌを計量してビーカーに入れた。
[Example 1]
First, as shown in Table 1, Se161.7 mg / L, Cu 0.5 mg / L, Pb 1.21 mg / L, Zn 4.3 mg / L, Fe 2.49 mg / L, As (arsenic) 682.3 mg / L, Hg 1 mL of selenium-containing wastewater containing 1.6 μg / L (mercury), pH-0.01, oxidation-reduction potential (ORP) (Ag / AgCl electrode) 370 mV was weighed into a beaker.
次に、このセレン含有排水に試薬（特級）の銅粉１０ｇを添加し、室温において直径３０ｍｍのプロペラ羽根を４００ｒｐｍで回転させて６０分間撹拌した。次に、未溶解成分と固体分を除去するため、５Ｃのろ紙を用いて吸引ろ過を行い、ろ液を分析した。その結果を表１に示す。 Next, 10 g of reagent (special grade) copper powder was added to the selenium-containing wastewater, and a propeller blade having a diameter of 30 mm was rotated at 400 rpm at room temperature and stirred for 60 minutes. Next, in order to remove undissolved components and solid components, suction filtration was performed using 5C filter paper, and the filtrate was analyzed. The results are shown in Table 1.
このようにして得られた銅が若干溶解した液１Ｌに試薬の鉄粉１０．６７ｇを添加した。この鉄粉の添加により電位が下がり、１５分間攪拌した後、吸引ろ過を行ない、ろ液を分析した。その結果を表１に示す。この表１に示すように、銅粉を添加した後に、脱銅するために鉄粉を添加すると、銅が除去されると同時にセレンも除去されていることがわかる。 Reagent iron powder 10.67 g was added to 1 L of a solution in which copper thus obtained was slightly dissolved. The potential was lowered by the addition of this iron powder, and after stirring for 15 minutes, suction filtration was performed and the filtrate was analyzed. The results are shown in Table 1. As shown in Table 1, it can be seen that when iron powder is added to remove copper after adding copper powder, copper is removed and selenium is removed at the same time.
［実施例２］
実施例１と同様にして得られた銅が若干溶解した液１Ｌに試薬の亜鉛粉１２．３３ｇを添加した。この亜鉛粉の添加により電位が下がり、１５分間攪拌した後、吸引ろ過を行ない、ろ液を分析した。その結果を表１に示す。この表１に示すように、銅粉を添加した後に、脱銅するために亜鉛粉を添加すると、銅が除去されると同時にセレンも除去されていることがわかる。
[Example 2]
12.33 g of reagent zinc powder was added to 1 L of a liquid in which copper obtained in the same manner as in Example 1 was slightly dissolved. The potential was lowered by the addition of the zinc powder, and after stirring for 15 minutes, suction filtration was performed and the filtrate was analyzed. The results are shown in Table 1. As shown in Table 1, it is understood that when zinc powder is added to remove copper after adding copper powder, selenium is removed at the same time as copper is removed.
［実施例３］
実施例１と同様のセレン含有排水に試薬のＣｕＳＯ４・５Ｈ２Ｏを１１．７９ｇ添加し、室温において直径３０ｍｍのプロペラ羽根を４００ｒｐｍで回転させて１５分間撹拌した。肉眼では全て溶解したように見えたが、５Ｃのろ紙を用いて吸引ろ過を行い、ろ液を分析した。その結果を表１に示す。この表１に示すように、銅イオンを添加するだけではセレンの濃度が変化していないのがわかる。
[Example 3]
11.79 g of the reagent CuSO 4 .5H 2 O was added to the same selenium-containing wastewater as in Example 1, and a propeller blade having a diameter of 30 mm was rotated at 400 rpm at room temperature and stirred for 15 minutes. Although all seemed to be dissolved with the naked eye, suction filtration was performed using 5C filter paper, and the filtrate was analyzed. The results are shown in Table 1. As shown in Table 1, it can be seen that the concentration of selenium does not change only by adding copper ions.
このようにして得られた硫酸銅が溶解した液１Ｌに試薬の鉄粉７．９１ｇを添加した。この鉄粉の添加により電位が下がり、１５分間攪拌した後、吸引ろ過を行ない、ろ液を分析した。その結果を表１に示す。この表１に示すように、硫酸銅を添加した後に、脱銅するために鉄粉を添加すると、銅が除去されると同時にセレンも除去されていることがわかる。 Reagent iron powder 7.91 g was added to 1 L of the solution in which the copper sulfate thus obtained was dissolved. The potential was lowered by the addition of this iron powder, and after stirring for 15 minutes, suction filtration was performed and the filtrate was analyzed. The results are shown in Table 1. As shown in Table 1, it can be seen that when iron powder is added to remove copper after adding copper sulfate, selenium is removed at the same time as copper is removed.
［実施例４］
実施例３と同様にして得られた硫酸銅が若解した液１Ｌに試薬の亜鉛粉９．２６ｇを添加した。この亜鉛粉の添加により電位が下がり、１５分間攪拌した後、吸引ろ過を行ない、ろ液を分析した。その結果を表１に示す。表１に示すように、硫酸銅を添加した後に、脱銅するために亜鉛粉を添加すると、銅が除去されると同時にセレンも除去されていることがわかる。
[Example 4]
9.26 g of reagent zinc powder was added to 1 L of a solution obtained by refining copper sulfate obtained in the same manner as in Example 3. The potential was lowered by the addition of the zinc powder, and after stirring for 15 minutes, suction filtration was performed and the filtrate was analyzed. The results are shown in Table 1. As shown in Table 1, it is understood that when zinc powder is added to remove copper after adding copper sulfate, copper is removed and selenium is also removed at the same time.
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