JP2019055350A - Processing method of tin-containing water - Google Patents
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本発明は、Ｓｎ含有水の処理方法に関し、特に、Ｓｎを含むめっき液などのＳｎを含有する廃液を処理する方法に関する。 The present invention relates to a method for treating Sn-containing water, and more particularly, to a method for treating a waste solution containing Sn such as a plating solution containing Sn.
従来、Ｓｎなどの重金属を含有する廃水を処理する方法として、廃水中に酸化剤を添加した後、アルカリを添加して重金属の水酸化物を析出させ、この水酸化物を含む廃水中に凝結剤を添加し、凝集剤を添加して凝集物を生成させた後、この凝集物を沈殿除去し、この凝集物を沈殿除去した廃水の上澄み液を濾過して、上澄み液中に残存する凝集物を除去し、さらに、この上澄み液中に残存する重金属を吸着して除去する方法が提案されている（例えば、特許文献１参照）。 Conventionally, as a method of treating wastewater containing heavy metals such as Sn, after adding an oxidizer to the wastewater, alkali is added to precipitate the hydroxide of the heavy metal and coagulate in the wastewater containing this hydroxide. After the agent is added and the flocculant is added to form an aggregate, the aggregate is precipitated and removed, and the supernatant liquid of the waste water from which the aggregate has been removed by filtration is filtered to leave the aggregate remaining in the supernatant liquid. There has been proposed a method for removing substances and further adsorbing and removing heavy metals remaining in the supernatant (for example, see Patent Document 1).
しかし、従来のＳｎ含有水の処理方法のように、Ｓｎ含有水中のＳｎをアルカリにより沈殿し、凝集剤を添加して凝集物を生成させた後に固液分離を行う方法では、固液分離後のろ液中のＳｎ濃度が高く、固液分離に使用したろ布の目詰まりの頻度が高いという問題がある。 However, as in the conventional method for treating Sn-containing water, in the method of solid-liquid separation after Sn in Sn-containing water is precipitated with an alkali and a flocculant is added to form an aggregate, There is a problem in that the Sn concentration in the filtrate is high and the frequency of clogging of the filter cloth used for solid-liquid separation is high.
したがって、本発明は、このような従来の問題点に鑑み、Ｓｎ含有水中のＳｎをアルカリにより沈殿させた後に固液分離を行う場合に、ろ液中のＳｎ濃度が低く、ろ布が目詰まりし難い、Ｓｎ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 a conventional problem, in the present invention, when solid-liquid separation is performed after Sn in Sn-containing water is precipitated by alkali, the Sn concentration in the filtrate is low and the filter cloth is clogged. It is an object of the present invention to provide a method for treating Sn-containing water which is difficult to do.
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、Ｓｎ含有水に活性炭を投入し、アルカリ液を添加した後、固液分離することにより、ろ液中のＳｎ濃度が低く、ろ布が目詰まりし難い、Ｓｎ含有水の処理方法を提供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 put activated carbon into Sn-containing water, added an alkaline liquid, and then solid-liquid separated, so that the Sn concentration in the filtrate is low, The present inventors have found that it is possible to provide a method for treating Sn-containing water, in which the filter cloth is hardly clogged, and the present invention has been completed.
すなわち、本発明によるＳｎ含有水の処理方法は、Ｓｎ含有水に活性炭を投入し、アルカリ液を添加した後、固液分離することを特徴とする。このＳｎ含有水の処理方法において、Ｓｎ含有水として、Ｓｎを含むめっき液の廃液を使用することができる。このＳｎ含有水は、酸性であるのが好ましく、ｐＨが６未満であるのがさらに好ましく、ｐＨが４以下であるのが最も好ましい。また、活性炭は、粉末状の活性炭であるのが好ましく、活性炭の投入量は、Ｓｎ含有水中のＳｎ１重量部に対して０．１〜３．０重量部であるのが好ましい。また、アルカリ液の添加により、活性炭を投入したＳｎ含有水のｐＨを６．０〜８．０にするのが好ましく、アルカリ液として、水酸化ナトリウム水溶液を使用するのが好ましい。さらに、固液分離は、フィルタープレスにより行うのが好ましい。 That is, the method for treating Sn-containing water according to the present invention is characterized in that activated carbon is added to Sn-containing water, an alkali solution is added, and then solid-liquid separation is performed. In this Sn-containing water treatment method, a plating solution waste solution containing Sn can be used as the Sn-containing water. The Sn-containing water is preferably acidic, more preferably has a pH of less than 6, and most preferably has a pH of 4 or less. Moreover, it is preferable that activated carbon is powdery activated carbon, and it is preferable that the input amount of activated carbon is 0.1-3.0 weight part with respect to Sn1 weight part in Sn containing water. Moreover, it is preferable to adjust the pH of Sn-containing water charged with activated carbon to 6.0 to 8.0 by adding an alkaline solution, and it is preferable to use an aqueous sodium hydroxide solution as the alkaline solution. Furthermore, the solid-liquid separation is preferably performed by a filter press.
本発明によれば、Ｓｎ含有水中のＳｎをアルカリにより沈殿させた後に固液分離を行う場合に、ろ液中のＳｎ濃度が低く、ろ布が目詰まりし難い、Ｓｎ含有水の処理方法を提供することができる。 According to the present invention, there is provided a method for treating Sn-containing water in which Sn concentration in a filtrate is low and filter cloth is not easily clogged when solid-liquid separation is performed after precipitation of Sn in Sn-containing water with an alkali. Can be provided.
本発明によるＳｎ含有水の処理方法の実施の形態では、Ｓｎ含有水に活性炭を投入し、アルカリ液を添加した後、固液分離する。 In the embodiment of the method for treating Sn-containing water according to the present invention, activated carbon is added to the Sn-containing water, and after adding an alkaline solution, solid-liquid separation is performed.
処理対象であるＳｎ含有水として、Ｓｎめっきに使用したＳｎめっき液（Ｓｎを含むめっき液）の廃液を使用することができる。このＳｎ含有水は、例えば、０．１〜１０ｇ／Ｌ程度（好ましくは０．５〜５ｇ／Ｌ程度）のＳｎと、アルキルスルホン酸、塩酸、硫酸などの酸を含み、１００質量ｐｐｍ以下（好ましくは５０質量ｐｐｍ以下）のＣｕ、Ｆｅ、Ｎｉなどを含んでもよい。このＳｎ含有水は、酸性であるのが好ましく、ｐＨが６未満であるのがさらに好ましく、ｐＨが４以下であるのが最も好ましい。 As the Sn-containing water to be treated, the waste solution of the Sn plating solution (plating solution containing Sn) used for Sn plating can be used. The Sn-containing water contains, for example, about 0.1 to 10 g / L (preferably about 0.5 to 5 g / L) of Sn and an acid such as alkylsulfonic acid, hydrochloric acid, sulfuric acid, and the like, and is 100 mass ppm or less ( Cu, Fe, Ni, etc., preferably 50 mass ppm or less) may be included. The Sn-containing water is preferably acidic, more preferably has a pH of less than 6, and most preferably has a pH of 4 or less.
活性炭は、粉末状の活性炭であるのが好ましい。この活性炭は、Ｓｎ含有水のｐＨが低い状態で投入するのが好ましく、ｐＨが３以下のＳｎ含有水に投入してもよい。活性炭の投入量は、Ｓｎ含有水中のＳｎ１重量部に対して０．１〜３．０重量部であるのが好ましく、０．２〜２．０重量部であるのがさらに好ましい。また、アルカリ液の添加により、活性炭を投入したＳｎ含有水のｐＨを好ましくは６．０〜８．０、さらに好ましくは６．５〜７．５にして、Ｓｎ含有水を中和するのが好ましい。アルカリ液として、水酸化ナトリウム水溶液などを使用することができるが、水酸化ナトリウム水溶液を使用するのが好ましい。なお、活性炭の投入と、アルカリ液の添加は、Ｓｎ含有水を撹拌しながら行うのが好ましい。また、固液分離は、フィルタープレスにより行うのが好ましい。 The activated carbon is preferably powdered activated carbon. This activated carbon is preferably added in a state where the pH of Sn-containing water is low, and may be added to Sn-containing water having a pH of 3 or less. The input amount of the activated carbon is preferably 0.1 to 3.0 parts by weight, and more preferably 0.2 to 2.0 parts by weight with respect to 1 part by weight of Sn in the Sn-containing water. The pH of the Sn-containing water charged with activated carbon is preferably 6.0 to 8.0, more preferably 6.5 to 7.5 by adding an alkaline solution to neutralize the Sn-containing water. preferable. A sodium hydroxide aqueous solution or the like can be used as the alkaline solution, but a sodium hydroxide aqueous solution is preferably used. The addition of activated carbon and the addition of the alkali solution are preferably performed while stirring the Sn-containing water. The solid-liquid separation is preferably performed by a filter press.
このようにＳｎ含有水に活性炭を投入してアルカリ液を添加した後に固液分離すれば、ろ液中のＳｎ濃度を（例えば１ｐｐｍ以下に）低下させて、ろ液の排水処理費用を削減することができるとともに、フィルタープレスなどにより固液分離する際にろ布が目詰まりし難くすることができる。なお、固液分離後の（沈殿物、水酸化Ｓｎ、活性炭などの）固形物は、有価物として回収することができる。 If the activated carbon is added to the Sn-containing water and the solid solution is separated after adding the alkali solution, the Sn concentration in the filtrate is reduced (for example, to 1 ppm or less), and the wastewater treatment cost of the filtrate is reduced. In addition, the filter cloth can be prevented from being clogged during solid-liquid separation by a filter press or the like. Note that solids (such as precipitates, hydroxylated Sn, and activated carbon) after solid-liquid separation can be recovered as valuables.
以下、本発明によるＳｎ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 Sn containing water by this invention is described in detail.
［実施例１］
２ｇ／ＬのＳｎと０．０２ｇ／ＬのＣｕと０．００６ｇ／ＬのＦｅとアルキルスルホン酸を含み、電気伝導率３０．０ｍＳ／ｃｍ、ｐＨ１．６３のＳｎ含有水５００Ｌを反応槽に入れ、Ｓｎ含有水を撹拌しながら、活性炭（和光純薬工業株式会社製の粉末活性炭（特級）（７４４０−４４−０）、粒径約５０μｍ）５００ｇ（１ｇ／Ｌ）（Ｓｎ１重量部に対して０．５重量部）を投入した後、４８質量％の水酸化ナトリウムを含む水酸化ナトリウム水溶液を添加して、Ｓｎ含有水のｐＨを調整し、Ｓｎ含有水のｐＨが７．００になったときに、水酸化ナトリウム水溶液の添加を停止して、攪拌を停止した。この溶液を（一部の沈殿物を除いて）フィルタープレス（日本エンバイロ工業株式会社製のＫＰＦ−３０Ｎ）内に圧入してろ過した。このフィルタープレス後のろ液中のＳｎ濃度をＩＣＰ発光分析装置により測定したところ、０．９０ｐｐｍと低かった。また、フィルタープレスのろ布の目詰まりはなかった。
[Example 1]
500 L of Sn-containing water containing 2 g / L of Sn, 0.02 g / L of Cu, 0.006 g / L of Fe, and alkylsulfonic acid, having an electric conductivity of 30.0 mS / cm and a pH of 1.63 is placed in the reaction vessel. While stirring Sn-containing water, activated carbon (powdered activated carbon (special grade) manufactured by Wako Pure Chemical Industries, Ltd. (7440-44-0), particle size of about 50 μm) 500 g (1 g / L) (based on 1 part by weight of Sn 0.5 parts by weight) was added, and a sodium hydroxide aqueous solution containing 48% by mass of sodium hydroxide was added to adjust the pH of the Sn-containing water, and the pH of the Sn-containing water became 7.00. Occasionally, the addition of aqueous sodium hydroxide was stopped and stirring was stopped. This solution was press-fitted into a filter press (KPF-30N manufactured by Nippon Enviro Kogyo Co., Ltd.) (excluding some precipitates) and filtered. When the Sn concentration in the filtrate after the filter press was measured with an ICP emission spectrometer, it was as low as 0.90 ppm. Moreover, the filter cloth of the filter press was not clogged.
［実施例２］
２ｇ／ＬのＳｎと０．０２ｇ／ＬのＣｕと０．００６ｇ／ＬのＦｅとアルキルスルホン酸を含み、電気伝導率２５．０ｍＳ／ｃｍ、ｐＨ１．７２のＳｎ含有水１０００Ｌを反応槽に入れ、Ｓｎ含有水を撹拌しながら、活性炭２ｋｇ（２ｇ／Ｌ）（Ｓｎ１重量部に対して１重量部）を投入した後、２５質量％の水酸化ナトリウム水溶液を添加して、Ｓｎ含有水のｐＨを調整し、Ｓｎ含有水のｐＨが７．００になったときに、水酸化ナトリウム水溶液の添加を停止して、攪拌を停止した。この溶液を実施例１と同様のフィルタープレス内に圧入してろ過した。このフィルタープレス後のろ液中のＳｎ濃度をＩＣＰ発光分析装置により測定したところ、０．１４ｐｐｍと低かった。また、フィルタープレスのろ布の目詰まりはなかった。
[Example 2]
2 g / L of Sn, 0.02 g / L of Cu, 0.006 g / L of Fe, and alkylsulfonic acid, electric conductivity of 25.0 mS / cm, pH 1.72 of Sn-containing water 1000 L was put into the reaction vessel. Then, while stirring Sn-containing water, 2 kg (2 g / L) of activated carbon (1 part by weight with respect to 1 part by weight of Sn) was added, and then a 25% by mass aqueous sodium hydroxide solution was added to adjust the pH of the Sn-containing water. When the pH of the Sn-containing water reached 7.00, the addition of the aqueous sodium hydroxide solution was stopped and the stirring was stopped. This solution was pressed into a filter press similar to that in Example 1 and filtered. When the Sn concentration in the filtrate after the filter press was measured by an ICP emission spectrometer, it was as low as 0.14 ppm. Moreover, the filter cloth of the filter press was not clogged.
［実施例３］
２ｇ／ＬのＳｎと０．０２ｇ／ＬのＣｕと０．００６ｇ／ＬのＦｅとアルキルスルホン酸を含み、電気伝導率１２．５ｍＳ／ｃｍ、ｐＨ１．９６のＳｎ含有水１０００Ｌを反応槽に入れ、Ｓｎ含有水を撹拌しながら、活性炭２ｋｇを投入した後、２５質量％の水酸化ナトリウム水溶液を添加して、Ｓｎ含有水のｐＨを調整し、Ｓｎ含有水のｐＨが６．９３になったときに、水酸化ナトリウム水溶液の添加を停止して、攪拌を停止した。この溶液を実施例１と同様のフィルタープレス内に圧入してろ過した。このフィルタープレス後のろ液中のＳｎ濃度をＩＣＰ発光分析装置により測定したところ、０．００ｐｐｍであった。また、フィルタープレスのろ布の目詰まりはなかった。
[Example 3]
1000 L of Sn-containing water containing 2 g / L Sn, 0.02 g / L Cu, 0.006 g / L Fe and alkylsulfonic acid, having an electric conductivity of 12.5 mS / cm and a pH of 1.96 is placed in a reaction vessel. After adding 2 kg of activated carbon while stirring Sn-containing water, the pH of Sn-containing water was adjusted to 6.93 by adding 25 mass% sodium hydroxide aqueous solution to adjust the pH of Sn-containing water. Occasionally, the addition of aqueous sodium hydroxide was stopped and stirring was stopped. This solution was pressed into a filter press similar to that in Example 1 and filtered. The Sn concentration in the filtrate after the filter press was measured by an ICP emission spectrometer, and found to be 0.00 ppm. Moreover, the filter cloth of the filter press was not clogged.
［比較例１］
２ｇ／ＬのＳｎと０．０２ｇ／ＬのＣｕと０．００６ｇ／ＬのＦｅとアルキルスルホン酸を含み、電気伝導率３３．６ｍＳ／ｃｍ、ｐＨ１．３８のＳｎ含有水５００Ｌを反応槽に入れ、Ｓｎ含有水を撹拌しながら、４８質量％の水酸化ナトリウム水溶液を添加して、Ｓｎ含有水のｐＨを調整し、この水酸化ナトリウム水溶液の添加中に、珪藻土０．７ｋｇを投入するとともに、ポリアクリルアミド系高分子からなる凝集剤１００ｍＬを投入し、Ｓｎ含有水のｐＨが７．２８になったときに、水酸化ナトリウム水溶液の添加を停止して、攪拌を停止した。この溶液を実施例１と同様のフィルタープレス内に圧入してろ過した。このフィルタープレス後のろ液中のＳｎ濃度をＩＣＰ発光分析装置により測定したところ、３．６ｐｐｍと高かった。なお、フィルタープレスのろ布の目詰まりはなかったが、実施例１〜３と比べて、ろ布上の固形物の粘度が高く、ろ布から固形物を剥ぎ取り難かったため、固液分離を繰り返すと、ろ布が目詰まりし易くなると考えられる。
[Comparative Example 1]
500 L of Sn-containing water containing 2 g / L of Sn, 0.02 g / L of Cu, 0.006 g / L of Fe and alkylsulfonic acid, having an electrical conductivity of 33.6 mS / cm and a pH of 1.38 is placed in a reaction vessel. While stirring the Sn-containing water, 48% by mass of sodium hydroxide aqueous solution was added to adjust the pH of the Sn-containing water, and 0.7 kg of diatomaceous earth was added during the addition of the sodium hydroxide aqueous solution. 100 mL of a flocculant composed of a polyacrylamide polymer was added, and when the pH of the Sn-containing water reached 7.28, the addition of the sodium hydroxide aqueous solution was stopped and stirring was stopped. This solution was pressed into a filter press similar to that in Example 1 and filtered. When the Sn concentration in the filtrate after the filter press was measured by an ICP emission spectrometer, it was as high as 3.6 ppm. In addition, although there was no clogging of the filter cloth of the filter press, compared with Examples 1-3, since the viscosity of the solid substance on a filter cloth was high and it was difficult to peel off a solid substance from a filter cloth, solid-liquid separation was carried out. If it repeats, it will be thought that a filter cloth becomes easy to clog.
［比較例２］
２ｇ／ＬのＳｎと０．０２ｇ／ＬのＣｕと０．００６ｇ／ＬのＦｅとアルキルスルホン酸を含み、電気伝導率３０．０ｍＳ／ｃｍ、ｐＨ１．６３のＳｎ含有水５００Ｌを反応槽に入れ、Ｓｎ含有水を撹拌しながら、４８質量％の水酸化ナトリウム水溶液を添加して、Ｓｎ含有水のｐＨを調整し、Ｓｎ含有水のｐＨが７．００になったときに、活性炭５００ｇを投入し、水酸化ナトリウム水溶液の添加を停止して、攪拌を停止した。この溶液を実施例１と同様のフィルタープレス内に圧入してろ過した。このフィルタープレス後のろ液中のＳｎ濃度をＩＣＰ発光分析装置により測定したところ、３．５ｐｐｍと高かった。なお、フィルタープレスのろ布の目詰まりはなかったが、実施例１〜３と比べて、ろ布上の固形物の粘度が高く、ろ布から固形物を剥ぎ取り難かったため、固液分離を繰り返すと、ろ布が目詰まりし易くなると考えられる。
[Comparative Example 2]
500 L of Sn-containing water containing 2 g / L of Sn, 0.02 g / L of Cu, 0.006 g / L of Fe, and alkylsulfonic acid, having an electric conductivity of 30.0 mS / cm and a pH of 1.63 is placed in the reaction vessel. While stirring Sn-containing water, 48% by mass of sodium hydroxide aqueous solution was added to adjust the pH of Sn-containing water, and when the pH of Sn-containing water reached 7.00, 500 g of activated carbon was added. Then, the addition of the aqueous sodium hydroxide solution was stopped and stirring was stopped. This solution was pressed into a filter press similar to that in Example 1 and filtered. When the Sn concentration in the filtrate after the filter press was measured by an ICP emission spectrometer, it was as high as 3.5 ppm. In addition, although there was no clogging of the filter cloth of the filter press, compared with Examples 1-3, since the viscosity of the solid substance on a filter cloth was high and it was difficult to peel off a solid substance from a filter cloth, solid-liquid separation was carried out. If it repeats, it will be thought that a filter cloth becomes easy to clog.
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